CN104090312B - Infrared metallic reflective coating of a kind of high adhesion force and preparation method thereof - Google Patents
Infrared metallic reflective coating of a kind of high adhesion force and preparation method thereof Download PDFInfo
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- CN104090312B CN104090312B CN201410369395.2A CN201410369395A CN104090312B CN 104090312 B CN104090312 B CN 104090312B CN 201410369395 A CN201410369395 A CN 201410369395A CN 104090312 B CN104090312 B CN 104090312B
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Abstract
The invention provides one and be coated with infrared metallic reflective coating of high adhesion force and preparation method thereof on the optical component substrates such as glass, metal and silicon crystal.The infrared metallic reflective coating of high adhesion force of the present invention comprises substrate, it is characterized in that evaporation has First Transition layer, occlusion adhesive linkage, metal level, Stress match layer, medium to strengthen protective seam and hard wear-resistant layer successively on substrate.Typical feature of the present invention is that film adhesion is good, reflectivity is high, abrasion-resistant, environmental suitability are strong, and possess higher threshold for resisting laser damage level, the military-civil photoelectron technical field such as infrared laser, refractive and reflective optical system, laser/infrared common road electro-optical equipment can be widely used in.
Description
Technical field
The present invention relates to one and be coated with infrared metallic reflective coating of high adhesion force and preparation method thereof on the optical components such as glass, metal and silicon crystal, belong to optical film technology field.
Background technology
Along with military electro-optical equipment is to the trend of multiband and multifunctional all development, the application of sweep type catoptron and catadioptric mirror is more and more extensive, and associated specifications also not only improves.Not only require that reflectance coating has good optics and mechanical property, and the threshold for resisting laser damage level of some strength must be possessed.On the other hand, infrared metallic reflective coating is at high-performance CO
2also extensive application on laser instrument, as the large scale catoptron in stacked laser instrument, adjusting-free rigging-angle cone catoptron, laser numerical control cutting equipment scanning reflection primary mirror etc.
At infrared band, the general mode being coated with protection type (or enhancement mode) metallic reflective coating that adopts realizes.At present, conventional protection type metallic reflectance coating (as Ag, Au etc.) is although can realize infrared band high reverse--bias, and reflectivity can reach more than 98%.But, because metallic diaphragm is softer, and and good chemisorption cannot be formed between substrate, to such an extent as to film adhesion and surface abrasion resistance to wipe performance often poor.This makes metallic mirror in assembling link palpus significant care, and is also unfavorable for clean clean when film surface is subject to polluting.In actual applications, metal level internal stress causes greatly that peeling comes off, moisture absorption burn into rete is unable to stand the problems such as wiping and is also happened occasionally, and these all directly affect serviceability and the reliability of catoptron.For polymorphic structure or large-sized catoptron, because the transverse direction of the oblique incidence effect in thin film growth process and rete internal stress is accumulated, often make the adhesion of metal level and substrate and surface abrasion resistance wipe performance and become poorer.
Based on this, for the development of the infrared metallic reflective coating of high adhesion force, be necessary to develop a kind of new film structure and preparation method thereof, to overcome above-mentioned many defects and to realize through engineering approaches application.
Summary of the invention
The invention provides a kind of infrared metallic reflective coating of high adhesion force be coated with on optical component surfaces such as glass, metal and silicon crystal and preparation method thereof.High adhesion force reflectance coating of the present invention comprises substrate, First Transition layer, occlusion adhesive linkage, metallic diaphragm, Stress match layer, medium enhancing protective seam and hard wear-resistant layer.By introducing occlusion adhesive linkage on First Transition layer basis, the adhesion of metal level and substrate is significantly promoted; By introducing Stress match layer and hard wear-resistant layer, making protection type (or enhancement mode) metallic reflective coating have good optical property and surperficial physical strength at infrared band, possessing adverse environment resistant performance to a certain degree simultaneously.
On the other hand, first ion beam etching clean substrate surfaces is adopted before evaporation rete, effectively peel off substrate (especially metallic substrates) surperficial organic contaminant and activating surface molecule (or atom), this be conducive to promote rete firmness with become film quality.
The invention provides one and be coated with infrared metallic reflective coating of high adhesion force and preparation method thereof at glass, crystal optical component surface.
Infrared metallic reflective coating, substrate (1) has following rete successively: First Transition layer (2), occlusion adhesive linkage (3), metallic diaphragm (4), Stress match layer (5), medium strengthen protective seam (6) and hard wear-resistant layer (7);
Substrate material (1) is glass or silicon crystal; First Transition layer (2) is formed through vacuum thermal evaporation by chromium, and adopt ion beam assisted depositing, and thickness is 20-60nm; Occlusion adhesive linkage (3) is made up of ultra-thin layer gold or silver layer and ultra-thin layers of chrome or layers of copper, and be followed successively by ultra-thin layer gold or silver layer on First Transition layer, ultra-thin layers of chrome or layers of copper, the thickness of ultra-thin layer gold or silver layer and ultra-thin layers of chrome or layers of copper is 2 ~ 20nm; Metallic diaphragm (4) be by purity be greater than 99.9% gold or silver adopt electron beam evaporation form, thickness is 100-200nm; Stress match layer (5) is by Al
2o
3or ZnS material electronics beam evaporation and being formed, thicknesses of layers is 18-35nm, adopts ion beam assisted depositing technique in evaporation process, makes Stress match layer show as compressive stress state; It is alternately be coated with by high and low refractive index material to be formed that medium strengthens protective seam (6), and adopts ion beam assisted depositing, and high-index material is TiO
2or ZnS or ZnSe, low-index material is YF
3or SiO
2; Hard wear-resistant layer (7) material selection Ta
2o
5, adopt ion beam assisted depositing in film forming procedure, thicknesses of layers is 15 ~ 30nm.
The thickness of First Transition layer (2) is 30-50nm, in occlusion adhesive linkage (3), the thickness of ultra-thin layer gold or silver layer and ultra-thin layers of chrome or layers of copper is 3 ~ 10nm, metallic diaphragm (4) thickness is 120-180nm, Stress match layer (5) thickness is 18-30nm, and hard wear-resistant layer (7) thickness is 20 ~ 30nm.
Occlusion adhesive linkage (3) is made up of ultra-thin layer gold and ultra-thin layers of chrome.
When Stress match layer material is Al
2o
3time, medium strengthens in protective seam (6), and high-index material is TiO
2, low-index material is SiO
2; When Stress match layer material is ZnS, medium strengthens in protective seam (6), and high-index material is ZnS or ZnSe, and low-index material is YF
3.
Hard, wear-resistant layer material replaces with HfO
2or Y
2o
3.
The preparation method of the infrared metallic reflective coating of high adhesion force comprises the steps:
(1) preliminary work: first use polishing fluid wiping one time, then clean with anhydrous mixed organic solvents, substrate is put into coating machine vaporization chamber, vacuumize and heat, heating-up temperature is 120 DEG C ~ 200 DEG C, and the time is 50-120min;
(2) ion beam etching cleaning: when background vacuum reaches 1.5 × 10
-3below Pa, simultaneously during the abundant heat penetration of substrate, open ion gun and carry out ion beam etching cleaning to substrate surface, working gas is argon gas, and screen pressure is 300-400V, 60-100mA with ion beam current, duration 6-15min, etch thicknesses 30 ~ 100nm;
(3) at the upper evaporation First Transition layer (2) of substrate (1), substrate adopt electron beam evaporation be coated with chromium rete, source parameters is arranged: 300-400V, 60-100mA, rate of sedimentation 0.1-0.3nm/s, employing purity is the chromium particulate material of 99.9%, carries out fritting degasification fully before evaporation;
(4) being coated with of adhesive linkage is engaged: chromium or the copper film material of selecting purity to be the gold of 99.99wt% or silver and purity to be 99.99wt%, adopt electron beam evaporation, and carry out abundant fritting before evaporation, film quality is affected into, the source parameters of depositing ultrathin gold or silver layer: 300-360V, 60-90mA to prevent splash, rate of sedimentation 0.1-0.5nm/s, next, switch electron gun and be coated with ultra-thin chromium or layers of copper, optimum configurations is identical with First Transition layer; If occlusion adhesive linkage selects copper film material, then need at the upper preplating one deck copper film of First Transition layer (2), optimum configurations is identical with First Transition layer, thickness 20-45nm;
(5) being coated with of metallic diaphragm: optimum configurations is identical with above-mentioned ultra-thin gold or silver film, at the initial stage of evaporation process, rate of sedimentation controls at about 0.3-0.4nm/s, after deposition thickness is greater than 100nm, progressively increase transmitter current, make rate of sedimentation slowly be increased to 1.4-1.6nm/s;
(6) being coated with of Stress match layer: regulate source parameters to be 80-150V, 50-70mA, changing coating process is automatic operational mode, and arrange and successively suspend, adopt electron beam evaporation ZnS or Al
2o
3block material, rate of sedimentation is set as 0.4-1.0nm/s, carries out electron beam fritting before evaporation;
(7) medium strengthens the preparation of protective seam: switch operating gas is that purity is greater than 99.9% oxygen, Stress match layer replaces evaporation low-refraction and high-index material respectively, thus form medium enhancement mode rete, wherein, low-refraction rate of sedimentation is 0.4-0.8nm/s, and the rate of sedimentation of high-index material is 0.20-0.45nm/s, and source parameters arranges and is: 200-350V, 70-100mA, carries out fritting fully before evaporation respectively;
(8) being coated with of hard wear-resistant layer: setting source parameters is: 300-360V, 60-90mA, and rate of sedimentation 0.1-0.5nm/s, carries out fritting degasification fully before evaporation;
(9) close ion gun and working gas and in-situ annealing under carrying out high vacuum condition, temperature is 240 DEG C ~ 300 DEG C, and temperature retention time is no less than 2 hours;
(10) continue to vacuumize, be progressively down to less than 80 DEG C to substrate temperature, open vaporization chamber pickup.
When occlusion adhesive linkage is coated with, the source parameters of depositing ultrathin gold or silver layer: 310-350V, 80-90mA, rate of sedimentation 0.2-0.4nm/s.
When Stress match layer is coated with, source parameters is 100-120V, 60-70mA, and rate of sedimentation is set as 0.7-0.9nm/s.
Namely beneficial effect the invention has the advantages that:
1) ion beam orientation etching substrate surface is adopted, effectively remove substrate surface organic contaminant and activating surface molecule (or atom), eliminate the defect seed that substrate surface is residual, thus effectively improve rete at on-chip adhesion and one-tenth film quality.
2) by introducing occlusion adhesive linkage on the basis of First Transition layer, making this rete and First Transition layer and metal interlevel form good physics and being engaged, and then substantially improving adhesion between metallic diaphragm and substrate.Meanwhile, be aided with vacuum in situ annealing process, make to spread fully between occlusal layer interior atoms (or molecule), affinity increases further, is thus also conducive to the adhesion promoting metal level and substrate.On the other hand, by vacuum annealing process, make metal layer itself defect reduce and crystallite dimension becomes large, this also helps simultaneously and improves metallic diaphragm optical property simultaneously.
3) consider that metal layer itself tension stress is comparatively large, by introducing compressive stress matching layer and carrying out ion gun process parameter optimizing, make matching layer and subsequent medium film produce compressive stress with magnitude, thus achieve stress elimination (or decline).The method efficiently solves the practical problems such as speckle caused by stress relief and protective seam (or dielectric coating series) be full of cracks after environmental suitability test.On the other hand, by introducing hard wear-resistant layer, make metallic reflective coating have good surperficial physical strength, moistureproof and anti-wear performance also significantly improves.
4) this preparation technology relies on common domestic filming equipment, and involved process is easy to transplant, and make infrared metallic reflective coating become film quality no longer strong depend-ence coating machine hardware state, yield rate significantly promotes.Meanwhile, in the present invention about the preparation method of " occlusion adhesive linkage " in the preparation of other rete to lifting film adhesion there is directive significance widely.
Accompanying drawing explanation
Fig. 1 is the infrared metallic reflecting film structure figure of high adhesion force;
Fig. 2 be large scale silicon crystal upper/long wave protection type gold reflectance coating actual measurement reflectance curve;
Fig. 3 is laser on K9 glass/infrared double-waveband enhancement mode silver reflectance coating curve (near infrared and medium-wave infrared wave band);
In figure, 1-substrate, 2-First Transition layer, 3-is engaged adhesive linkage, 4-metallic diaphragm, 5-Stress match layer, and 6-medium strengthens protective seam, 7-hard wear-resistant layer
Embodiment
The infrared metallic reflective coating of a kind of high adhesion force involved in the present invention realizes on domestic southern light ZZS800 type vacuum coating equipment.This Equipments Setting has φ 120mm wide beam Kaufman ion source, electron gun evaporation system, MDC360 crystalline substance control instrument etc.
Embodiment 1:
A kind of medium wave and LONG WAVE INFRARED highly reflecting films, substrate material is monocrystalline silicon, size 110 × 180 × 14mm.Technical requirement is as follows:
incident angle 45 °.The adhesion that plated film print is disposable to be specified by GJB2485-1995 and moderate friction test.
First, carry out film structure optimal design according to above-mentioned technical requirement, result is as follows:
Sub/aCr/bM/cAu/dZnS/eYF
3/fZnS/gTa
2O
5/Air
Wherein, a-f is respectively rete physical thickness, M be ultra-thin layers of chrome form with ultra-thin layer gold be engaged adhesive linkage, its physical thickness is respectively 3.0nm and 5.5nm.Other thickness is followed successively by: a-30nm; C-130nm; D-18nm; E-125nm; F-60nm, g-20nm.
Preparation process is specifically implemented as follows:
(1) preliminary work: first wipe roughly one time with special-purpose polishing liquid, clean with anhydrous mixed organic solvents again, then check whether the smooth finish standard conformed with the regulations by the method for breathing out, after qualified, put into coating machine vaporization chamber, vacuumize and heat eyeglass, opening support rotates.Heating-up temperature is set as 180 DEG C, and heat penetration 85 minutes.
(2) ion beam etching cleaning: when reaching base vacuum 1.5 × 10
-3during Pa, open ion gun and carry out Ions Bombardment to substrate surface, working gas is high-purity argon gas (4N).Optimum configurations: screen pressure and ion beam current 330V/90mA, 8 minutes duration; Etching physical thickness is about 35nm.
(3) on substrate, adopt electron beam evaporation to be coated with First Transition layer (chromium film), physical thickness 30nm.Source parameters is arranged: 310V/85mA, rate of sedimentation 0.15nm/s.Employing purity is the chromium particulate material of 99.9%, carries out fritting degasification fully before evaporation.
(4) be engaged being coated with of adhesive linkage: select purity be 99.99% golden coating materials, adopt electron beam evaporation, and carry out abundant fritting before evaporation, affect into film quality to prevent splash.The physical thickness of ultra-thin layer gold is 5.5nm, source parameters: 310V/85mA.In evaporation process, rate of sedimentation controls at about 0.4nm/s.Next, switch electron gun and be coated with ultra-thin layers of chrome, optimum configurations is identical with same First Transition layer, and deposition physical thickness is 3.0nm.
(5) being coated with of golden membranous layer: optimum configurations is identical with above-mentioned ultra-thin golden membranous layer, and at the initial stage of evaporation process, rate of sedimentation controls at about 0.4nm/s.After deposition thickness is greater than 100nm, progressively increases transmitter current, make rate of sedimentation slowly be increased to about 1.5nm/s.
(6) being coated with of Stress match layer: adjustment source parameters is 110V/60mA, and changing coating process is automatic operational mode, and arrange and successively suspend.Adopt electron beam evaporation ZnS block material, rate of sedimentation is set as 0.8nm/s.Carry out electron beam fritting before evaporation, thicknesses of layers is set as 18nm.
(7) medium strengthens being coated with of protective seam: adjustment source parameters is 24V/40mA, Evaporation preparation medium protective layer.Adopt electron beam evaporation YF
3material, must carry out fritting fully, with antispray before evaporation.In evaporation process, rate of sedimentation is set as 0.6nm/s, and rete physical thickness is set as 165nm.Next, plated film high refractive index layer ZnS, technological parameter is identical with being coated with of Stress match layer, and thickness is 60nm.
(8) being coated with of hard wear-resistant layer: setting source parameters is 280V/80mA, rate of sedimentation 0.25nm/s, and physical thickness is 20nm.Fritting degasification is fully carried out before evaporation.
(9) ion gun and working gas is closed and in-situ annealing under carrying out high vacuum condition.Substrate baking temperature is 260 DEG C, temperature retention time 3 hours.
(10) continue to vacuumize, be down to less than 80 DEG C to substrate temperature, open vaporization chamber pickup.
Embodiment 2:
A kind of laser/infrared double-waveband highly reflecting films, substrate material is K9 glass, size 100 × 140 × 12mm.Technical requirement is as follows:
incident angle 10 ° ~ 60 °.The adhesion that plated film print must be specified by GJB2485-1995 and moderate friction test, and threshold for resisting laser damage level is greater than 300MW/cm
2.
First, carry out film structure optimal design according to above-mentioned technical requirement, result is as follows:
Sub|aCr/bM/cAg/dAl
2O
3/eSiO
2/fTiO
2/gSiO
2/hTiO
2/iTa
2O
5/Air
Wherein, a-f is respectively rete physical thickness, M be ultra-thin layers of copper form with ultra-thin silver layer be engaged adhesive linkage, its physical thickness is respectively 8.5nm and 13.0nm.Other thickness is followed successively by: a-30nm; C-130nm; D-35nm; E-28nm; F-71.8nm; G-53.9nm; H-54.2nm; I-20nm.
Preparation process is specifically implemented as follows:
(1) preliminary work: first wipe roughly one time with special-purpose polishing liquid, then clean with anhydrous mixed organic solvents, then with method inspection of breathing out, puts into coating machine vaporization chamber, vacuumizes and heat eyeglass after qualified.Heating-up temperature is set as 140 DEG C, and heat penetration 75 minutes.
(2) ion beam etching cleaning: when reaching base vacuum 1.5 × 10
-3during Pa, open ion gun and carry out Ions Bombardment to substrate surface, working gas is high-purity argon gas (4N).Optimum configurations: screen pressure and ion beam current 330V/90mA, 10 minutes duration; Etching physical thickness is about 50nm.
(3) on substrate, electron beam evaporation is adopted to be coated with chromium rete, physical thickness 30nm.Source parameters is arranged: 310V/85mA, rate of sedimentation 0.15nm/s.Employing purity is the chromium particulate material of 99.9%, carries out fritting degasification fully before evaporation.
(4) be engaged being coated with of adhesive linkage: select purity be 99.99% copper and silverskin material, adopt electron beam evaporation, and carry out abundant fritting before evaporation, affect into film quality to prevent splash.First the layers of copper that pre-deposition 25nm is thick, source parameters: 310V/85mA, rate of sedimentation 0.2nm/s.Then depositing ultrathin silver layer, rate of sedimentation controls at about 0.5nm/s, and deposit thickness is 13.0nm.Next, switch electron gun and be coated with ultra-thin layers of copper, optimum configurations is identical with preplating layers of copper, and deposition physical thickness is 8.5nm.
(5) ion gun and working gas is closed, when vacuum tightness reaches 1.5 × 10
-3pa and following time, occlusion adhesive linkage on adopt electron beam evaporation to be coated with Ag rete fast, thickness is 130nm.Carry out rapid premelter before evaporation, open to molten bath.During evaporation, Emission Current In An Electron Gun is set as 205mA.
(6) ion gun is opened, evaporation Stress match layer Al on metallic diaphragm
2o
3.Changing coating process is automatic operational mode, and source parameters is arranged: 250V/70mA, rate of sedimentation 0.2nm/s.Fritting is fully carried out before evaporation.
(7) switch operating gas is that purity is greater than 99.9% oxygen, and Stress match layer replaces evaporation low-refraction SiO respectively
2with high-index material TiO
2, thus form enhancement mode dielectric coating series.Wherein, SiO
2with TiO
2rate of sedimentation be respectively 0.6nm/s and 0.35nm/s, source parameters arrange be: 300V/85mA.Fritting is fully carried out respectively before evaporation.
(8) being coated with of hard wear-resistant layer: setting source parameters is 330V/85mA, rate of sedimentation 0.25nm/s, and physical thickness is 20nm.Fritting degasification is fully carried out before evaporation.
(9) close ion gun and working gas and in-situ annealing under carrying out high vacuum condition, substrate baking temperature is raised to 240 DEG C, temperature retention time 3 hours.
(10) continue pumping high vacuum, be progressively down to less than 80 DEG C to substrate temperature, open vaporization chamber pickup.
Claims (7)
1. the infrared metallic reflective coating of high adhesion force, is characterized in that: on substrate (1), have following rete successively: First Transition layer (2), occlusion adhesive linkage (3), metallic diaphragm (4), Stress match layer (5), medium strengthen protective seam (6) and hard wear-resistant layer (7);
Substrate (1) material is glass or silicon crystal; First Transition layer (2) is formed through vacuum thermal evaporation by chromium, and adopt ion beam assisted depositing, and thickness is 20-60nm; Occlusion adhesive linkage (3) is made up of ultra-thin layer gold or silver layer and ultra-thin layers of chrome or layers of copper, and be followed successively by ultra-thin layer gold or silver layer on First Transition layer, ultra-thin layers of chrome or layers of copper, the thickness of ultra-thin layer gold or silver layer and ultra-thin layers of chrome or layers of copper is 2 ~ 20nm; Metallic diaphragm (4) be by purity be greater than 99.9% gold or silver adopt electron beam evaporation form, thickness is 100-200nm; Stress match layer (5) is by Al
2o
3or ZnS material electronics beam evaporation and being formed, thicknesses of layers is 18-35nm, adopts ion beam assisted depositing technique in evaporation process, makes Stress match layer show as compressive stress state; It is alternately be coated with by high and low refractive index material to be formed that medium strengthens protective seam (6), and adopts ion beam assisted depositing, and high-index material is TiO
2or ZnS or ZnSe, low-index material is YF
3or SiO
2; Hard wear-resistant layer (7) material selection Ta
2o
5, adopt ion beam assisted depositing in film forming procedure, thicknesses of layers is 15 ~ 30nm;
When Stress match layer material is Al
2o
3time, medium strengthens in protective seam (6), and high-index material is TiO
2, low-index material is SiO
2; When Stress match layer material is ZnS, medium strengthens in protective seam (6), and high-index material is ZnS or ZnSe, and low-index material is YF
3.
2. infrared metallic reflective coating according to claim 1, it is characterized in that: the thickness of First Transition layer (2) is 30-50nm, in occlusion adhesive linkage (3), the thickness of ultra-thin layer gold or silver layer and ultra-thin layers of chrome or layers of copper is 3 ~ 10nm, metallic diaphragm (4) thickness is 120-180nm, Stress match layer (5) thickness is 18-30nm, and hard wear-resistant layer (7) thickness is 20 ~ 30nm.
3. infrared metallic reflective coating according to claim 2, is characterized in that: occlusion adhesive linkage (3) is made up of ultra-thin layer gold and ultra-thin layers of chrome.
4. infrared metallic reflective coating according to claim 2, is characterized in that: hard, wear-resistant layer material replaces with HfO
2or Y
2o
3.
5. prepare a method for the infrared metallic reflective coating of high adhesion force described in claim 1-4 any one, it is characterized in that, the method comprises the steps:
(1) preliminary work: first use polishing fluid wiping one time, then clean with anhydrous mixed organic solvents, substrate is put into coating machine vaporization chamber, vacuumize and heat, heating-up temperature is 120 DEG C ~ 200 DEG C, and the time is 50-120min;
(2) ion beam etching cleaning: when background vacuum reaches 1.5 × 10
-3below Pa, simultaneously during the abundant heat penetration of substrate, open ion gun and carry out ion beam etching cleaning to substrate surface, working gas is argon gas, and screen pressure is 300-400V, 60-100mA with ion beam current, duration 6-15min, etch thicknesses 30 ~ 100nm;
(3) at the upper evaporation First Transition layer (2) of substrate (1), substrate adopt electron beam evaporation be coated with chromium rete, source parameters is arranged: 300-400V, 60-100mA, rate of sedimentation 0.1-0.3nm/s, employing purity is the chromium particulate material of 99.9%, carries out fritting degasification fully before evaporation;
(4) being coated with of adhesive linkage is engaged: chromium or the copper film material of selecting purity to be the gold of 99.99wt% or silver and purity to be 99.99wt%, adopt electron beam evaporation, and carry out abundant fritting before evaporation, film quality is affected into, the source parameters of depositing ultrathin gold or silver layer: 300-360V, 60-90mA to prevent splash, rate of sedimentation 0.1-0.5nm/s, next, switch electron gun and be coated with ultra-thin chromium or layers of copper, optimum configurations is identical with First Transition layer; If occlusion adhesive linkage selects copper film material, then need at the upper preplating one deck copper film of First Transition layer (2), optimum configurations is identical with First Transition layer, thickness 20-45nm;
(5) being coated with of metallic diaphragm: optimum configurations is identical with above-mentioned ultra-thin gold or silver film, at the initial stage of evaporation process, rate of sedimentation controls at 0.3-0.4nm/s, after deposition thickness is greater than 100nm, progressively increase transmitter current, make rate of sedimentation slowly be increased to 1.4-1.6nm/s;
(6) being coated with of Stress match layer: regulate source parameters to be 80-150V, 50-70mA, changing coating process is automatic operational mode, and arrange and successively suspend, adopt electron beam evaporation ZnS or Al
2o
3block material, rate of sedimentation is set as 0.4-1.0nm/s, carries out electron beam fritting before evaporation;
(7) medium strengthens the preparation of protective seam: switch operating gas is that purity is greater than 99.9% oxygen, Stress match layer replaces evaporation low-refraction and high-index material respectively, thus form medium enhancement mode rete, wherein, low-refraction rate of sedimentation is 0.4-0.8nm/s, and the rate of sedimentation of high-index material is 0.20-0.45nm/s, and source parameters arranges and is: 200-350V, 70-100mA, carries out fritting fully before evaporation respectively;
(8) being coated with of hard wear-resistant layer: setting source parameters is: 300-360V, 60-90mA, and rate of sedimentation 0.1-0.5nm/s, carries out fritting degasification fully before evaporation;
(9) close ion gun and working gas and in-situ annealing under carrying out high vacuum condition, temperature is 240 DEG C ~ 300 DEG C, and temperature retention time is no less than 2 hours;
(10) continue to vacuumize, be progressively down to less than 80 DEG C to substrate temperature, open vaporization chamber pickup.
6. method according to claim 5, is characterized in that: when occlusion adhesive linkage is coated with, the source parameters of depositing ultrathin gold or silver layer: 310-350V, 80-90mA, rate of sedimentation 0.2-0.4nm/s.
7. method according to claim 5, is characterized in that: when Stress match layer is coated with, source parameters is 100-120V, 60-70mA, and rate of sedimentation is set as 0.7-0.9nm/s.
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