CN104090312A - Infrared metal reflecting film with high adhesive force and manufacturing method thereof - Google Patents
Infrared metal reflecting film with high adhesive force and manufacturing method thereof Download PDFInfo
- Publication number
- CN104090312A CN104090312A CN201410369395.2A CN201410369395A CN104090312A CN 104090312 A CN104090312 A CN 104090312A CN 201410369395 A CN201410369395 A CN 201410369395A CN 104090312 A CN104090312 A CN 104090312A
- Authority
- CN
- China
- Prior art keywords
- layer
- evaporation
- ultra
- sedimentation
- substrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
The invention provides an infrared metal reflecting film with high adhesive force and a manufacturing method thereof, wherein the infrared metal reflecting film with high adhesive force is plated on substrates of optical components such as glass, metal and silicon crystals. The infrared metal reflecting film with high adhesive force comprises a substrate, and is characterized in that a first transition layer, a holding-on bonding layer, a metal layer, a stress matching layer, a dielectric enhancement protecting layer and a hard wear-resistant layer are sequentially arranged on the substrate in an evaporation mode. The infrared metal reflecting film has the advantages of being good in film adhesive force, high in reflectivity, resistant to wear and high in environmental suitability, has a high laser damage resistance threshold value level, and can be widely applied to military and civilian photoelectron technical fields such as infrared lasers, refraction-reflection type optical systems and laser/infrared universal photoelectric equipment.
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 correlation technique requires also not only to improve.Not only require reflectance coating to there is good optics and mechanical property, and must possess the threshold for resisting laser damage level of some strength.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 that is 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 the high reflection of infrared band, and reflectivity can reach more than 98%.But, because metallic diaphragm is softer, and and substrate between cannot form good chemisorption, to such an extent as to that film adhesion and surface abrasion resistance are wiped performance is often poor.This makes the metallic mirror must significant care in assembling link, and film surface is also unfavorable for while being subject to polluting clean clean.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, due to the horizontal accumulation of the oblique incidence effect in thin film growth process and rete internal stress, often make the adhesion of metal level and substrate and surface abrasion resistance wiping performance 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 being 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 that substrate, First Transition layer, interlock adhesive linkage, metallic diaphragm, Stress match layer, medium strengthen protective seam and hard wear-resistant layer.By introduce interlock 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, make protection type (or enhancement mode) metallic reflective coating there is good optical property and surperficial physical strength at infrared band, possess adverse environment resistant performance to a certain degree simultaneously.
On the other hand, before evaporation rete, first adopt ion beam etching clean substrate surfaces, effectively peel off substrate (especially metallic substrates) surperficial organic contaminant activating surface molecule (or atom), this firmness that is conducive to promote rete with become film quality.
The invention provides one and be coated with infrared metallic reflective coating of high adhesion force and preparation method thereof on glass, silicon crystal optical component surface.
Infrared metallic reflective coating has successively following rete on substrate (1): First Transition layer (2), interlock 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 to be formed through vacuum thermal evaporation by chromium, and adopts ion beam assisted depositing, and thickness is 20-60nm; Interlock adhesive linkage (3) is made up of ultra-thin gold layer or silver layer and ultra-thin chromium layer or copper layer, is followed successively by ultra-thin gold layer or silver layer on First Transition layer, ultra-thin chromium layer or copper layer, and the thickness of ultra-thin gold layer or silver layer and ultra-thin chromium layer or copper layer 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 forming, 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 to be alternately coated with and to form by high and low refractive index material 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, in film forming procedure, adopting ion beam assisted depositing, thicknesses of layers is 15～30nm.
The thickness of First Transition layer (2) is 30-50nm, in interlock adhesive linkage (3), the thickness of ultra-thin gold layer or silver layer and ultra-thin chromium layer or copper layer 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.
Interlock adhesive linkage (3) is made up of ultra-thin gold layer and ultra-thin chromium layer.
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; In the time that 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 with anhydrous mixed organic solvents cleaning, 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 cleans: when base vacuum degree reaches 1.5 × 10
-3below Pa, when the abundant heat penetration of while substrate, open ion gun substrate surface is carried out to ion beam etching cleaning, working gas is argon gas, and it is 300-400V that screen is pressed with ion beam current, 60-100mA, duration 6-15min, etch thicknesses 30～100nm;
(3) at the upper evaporation First Transition layer (2) of substrate (1), on substrate, adopt electron beam evaporation to be coated with chromium rete, source parameters arranges: 300-400V, 60-100mA, rate of sedimentation 0.1-0.3nm/s, adopt the chromium particulate material that purity is 99.9%, before evaporation, carry out fritting degasification fully;
(4) being coated with of interlock adhesive linkage: selecting purity is gold or chromium or the copper film material silver-colored and that purity is 99.99wt% of 99.99wt%, adopt electron beam evaporation, and carry out abundant fritting before evaporation, affect into film quality to prevent splash, the source parameters of depositing ultrathin gold or silver layer: 300-360V, 60-90mA, rate of sedimentation 0.1-0.5nm/s, next, switch electron gun and be coated with ultra-thin chromium or copper layer, parameter setting is identical with First Transition layer; If interlock adhesive linkage is selected copper film material, need be at the upper preplating one deck copper film of First Transition layer (2), parameter setting is identical with First Transition layer, thickness 20-45nm;
(5) being coated with of metallic diaphragm: parameter setting is identical with above-mentioned ultra-thin gold or silver film, at the initial stage of evaporation process, rate of sedimentation is controlled at 0.3-0.4nm/s left and right, 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: adjusting source parameters is 80-150V, 50-70mA, changing coating process is automatic operational mode, and successively time-out is set, and adopts electron beam evaporation ZnS or Al
2o
3piece 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, on Stress match layer, replace respectively evaporation low-refraction and high-index material, thereby 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 setting is: 200-350V, 70-100mA, carries out respectively fritting fully before evaporation;
(8) being coated with of hard wear-resistant layer: setting source parameters is: 300-360V, 60-90mA, rate of sedimentation 0.1-0.5nm/s, carries out fritting degasification fully before evaporation;
(9) close ion gun and working gas and carry out in-situ annealing under 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 below 80 DEG C to substrate temperature, open vaporization chamber pickup.
When interlock 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.
Beneficial effect the invention has the advantages that:
1) adopt the directed etching substrate surface of ion beam, effectively remove substrate surface organic contaminant activating surface molecule (or atom), eliminate the residual defect seed of substrate surface, thereby effectively promoted rete at on-chip adhesion and become film quality.
2), by introducing interlock adhesive linkage on the basis at First Transition layer, make this rete and First Transition layer and metal interlevel form good physics interlock, and then substantially promoted adhesion between metallic diaphragm and substrate.Meanwhile, be aided with vacuum in situ annealing process, make diffusion fully between the inner atom of occlusal layer (or molecule), affinity further increases, thereby is also conducive to promote the adhesion of metal level and substrate.On the other hand, by vacuum annealing process, make the minimizing of metal level inherent vice and crystallite dimension become large, this also helps simultaneously and improves metallic diaphragm optical property simultaneously.
3) consider that the inner tension stress of metal level is larger, by introducing compressive stress matching layer and carrying out ion gun process parameter optimizing, make matching layer and subsequent medium film produce the compressive stress with magnitude, thereby realized stress elimination (or decline).The method has solved the practical problems such as speckle and protective seam (or dielectric coating series) be full of cracks due to the rear stress relief of environmental suitability test effectively.On the other hand, by introducing hard wear-resistant layer, make metallic reflective coating have good surperficial physical strength, protection against the tide and anti-wear performance also obviously improve.
4) this preparation technology relies on common domestic filming equipment, and related process is easy to transplant, and makes infrared metallic reflective coating become film quality no longer strongly to rely on coating machine hardware state, and yield rate significantly promotes.Meanwhile, in the present invention, the preparation method about " interlock adhesive linkage " has directive significance widely to promoting film adhesion in the preparation of other rete.
Brief description of the drawings
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 K9 laser/infrared double-waveband on glass enhancement mode silver reflectance coating curve (near infrared and medium-wave infrared wave band);
In figure, 1-substrate, 2-First Transition layer, 3-interlock adhesive linkage, 4-metallic diaphragm, 5-Stress match layer, 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 is realized on domestic southern light ZZS800 type vacuum coating equipment.This equipment disposes φ 120mm wide beam Kaufman ion source, electron gun evaporation system, the brilliant control of MDC360 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:
45 ° of incident angles.The disposable adhesion specifying by GJB2485-1995 of plated film print 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, and M is the interlock adhesive linkage of ultra-thin chromium layer and ultra-thin gold layer composition, and 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 one time with special-purpose polishing liquid is rough, clean with anhydrous mixed organic solvents, the smooth finish standard then whether conforming with the regulations with the method inspection of breathing out, puts into coating machine vaporization chamber after qualified again, 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 cleans: when reaching base vacuum 1.5 × 10
-3when Pa, open ion gun substrate surface is carried out to Ions Bombardment, working gas is high-purity argon gas (4N).Parameter arranges: screen is pressed and ion beam current 330V/90mA, 8 minutes duration; The about 35nm of etching physical thickness.
(3) on substrate, adopt electron beam evaporation to be coated with First Transition layer (chromium film), physical thickness 30nm.Source parameters arranges: 310V/85mA, rate of sedimentation 0.15nm/s.Adopt the chromium particulate material that purity is 99.9%, before evaporation, carry out fritting degasification fully.
(4) being coated with of interlock adhesive linkage: selecting purity is 99.99% golden coating materials, adopts electron beam evaporation, and carries out abundant fritting before evaporation, affects into film quality to prevent splash.The physical thickness of ultra-thin gold layer is 5.5nm, source parameters: 310V/85mA.In evaporation process, rate of sedimentation is controlled at 0.4nm/s left and right.Next, switch electron gun and be coated with ultra-thin chromium layer, parameter setting is identical with same First Transition layer, and deposition physical thickness is 3.0nm.
(5) being coated with of golden membranous layer: parameter setting is identical with above-mentioned ultra-thin golden membranous layer, at the initial stage of evaporation process, rate of sedimentation is controlled at 0.4nm/s left and right.After deposition thickness is greater than 100nm, progressively increase transmitter current, make rate of sedimentation slowly be increased to 1.5nm/s left and right.
(6) being coated with of Stress match layer: adjusting source parameters is 110V/60mA, changing coating process is automatic operational mode, and successively time-out is set.Adopt electron beam evaporation ZnS piece material, rate of sedimentation is set as 0.8nm/s.Before evaporation, carry out electron beam fritting, thicknesses of layers is set as 18nm.
(7) medium strengthens being coated with of protective seam: adjusting source parameters is 24V/40mA, Evaporation preparation medium protective layer.Adopt electron beam evaporation YF
3material, must carry out fritting fully before evaporation, with antispray.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, physical thickness is 20nm.Before evaporation, carry out fritting degasification fully.
(9) close ion gun and working gas and carry out in-situ annealing under high vacuum condition.Substrate baking temperature is 260 DEG C, temperature retention time 3 hours.
(10) continue to vacuumize, be down to below 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:
10 °～60 ° of incident angles.The adhesion that plated film print must specify 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, and M is the interlock adhesive linkage of super thin copper layer and ultra-thin silver layer composition, and 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 one time with special-purpose polishing liquid is rough, then with anhydrous mixed organic solvents cleaning, then with the method inspection of breathing out, put into coating machine vaporization chamber after qualified, vacuumize and heat eyeglass.Heating-up temperature is set as 140 DEG C, and heat penetration 75 minutes.
(2) ion beam etching cleans: when reaching base vacuum 1.5 × 10
-3when Pa, open ion gun substrate surface is carried out to Ions Bombardment, working gas is high-purity argon gas (4N).Parameter arranges: screen is pressed and ion beam current 330V/90mA, 10 minutes duration; The about 50nm of etching physical thickness.
(3) on substrate, adopt electron beam evaporation to be coated with chromium rete, physical thickness 30nm.Source parameters arranges: 310V/85mA, rate of sedimentation 0.15nm/s.Adopt the chromium particulate material that purity is 99.9%, before evaporation, carry out fritting degasification fully.
(4) being coated with of interlock adhesive linkage: selecting purity is 99.99% copper and silverskin material, adopts electron beam evaporation, and carries out abundant fritting before evaporation, affects into film quality to prevent splash.First the copper layer that pre-deposition 25nm is thick, source parameters: 310V/85mA, rate of sedimentation 0.2nm/s.Then depositing ultrathin silver layer, rate of sedimentation is controlled at 0.5nm/s left and right, and deposit thickness is 13.0nm.Next, switch electron gun and be coated with super thin copper layer, parameter setting is identical with pre-copper plate, and deposition physical thickness is 8.5nm.
(5) close ion gun and working gas, when vacuum tightness reaches 1.5 × 10
-3pa and when following adopts electron beam evaporation to be coated with fast Ag rete on interlock adhesive linkage, and thickness is 130nm.Before evaporation, carry out quick fritting, open to molten bath.When evaporation, Emission Current In An Electron Gun is set as 205mA.
(6) open ion gun, evaporation Stress match layer Al on metallic diaphragm
2o
3.Changing coating process is automatic operational mode, source parameters setting: 250V/70mA, rate of sedimentation 0.2nm/s.Before evaporation, carry out fritting fully.
(7) switch operating gas is that purity is greater than 99.9% oxygen, replaces respectively evaporation low-refraction SiO on Stress match layer
2with high-index material TiO
2thereby, form enhancement mode dielectric coating series.Wherein, SiO
2with TiO
2rate of sedimentation be respectively 0.6nm/s and 0.35nm/s, source parameters setting is: 300V/85mA.Before evaporation, carry out respectively fritting fully.
(8) being coated with of hard wear-resistant layer: setting source parameters is 330V/85mA, rate of sedimentation 0.25nm/s, physical thickness is 20nm.Before evaporation, carry out fritting degasification fully.
(9) close ion gun and working gas and carry out in-situ annealing under 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 below 80 DEG C to substrate temperature, open vaporization chamber pickup.
Claims (8)
1. the infrared metallic reflective coating of high adhesion force, is characterized in that: on substrate (1), have successively following rete: First Transition layer (2), interlock 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 to be formed through vacuum thermal evaporation by chromium, and adopts ion beam assisted depositing, and thickness is 20-60nm; Interlock adhesive linkage (3) is made up of ultra-thin gold layer or silver layer and ultra-thin chromium layer or copper layer, is followed successively by ultra-thin gold layer or silver layer on First Transition layer, ultra-thin chromium layer or copper layer, and the thickness of ultra-thin gold layer or silver layer and ultra-thin chromium layer or copper layer 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 forming, 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 to be alternately coated with and to form by high and low refractive index material 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, in film forming procedure, adopting ion beam assisted depositing, thicknesses of layers is 15～30nm.
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 interlock adhesive linkage (3), the thickness of ultra-thin gold layer or silver layer and ultra-thin chromium layer or copper layer 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: interlock adhesive linkage (3) is made up of ultra-thin gold layer and ultra-thin chromium layer.
4. infrared metallic reflective coating according to claim 3, is characterized in that: 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; In the time that 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.
5. infrared metallic reflective coating according to claim 2, is characterized in that: hard, wear-resistant layer material replaces with HfO
2or Y
2o
3.
6. a method of preparing the infrared metallic reflective coating of high adhesion force described in claim 1-4, is characterized in that, the method comprises the steps:
(1) preliminary work: first use polishing fluid wiping one time, then with anhydrous mixed organic solvents cleaning, 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 cleans: when base vacuum degree reaches 1.5 × 10
-3below Pa, when the abundant heat penetration of while substrate, open ion gun substrate surface is carried out to ion beam etching cleaning, working gas is argon gas, and it is 300-400V that screen is pressed with ion beam current, 60-100mA, duration 6-15min, etch thicknesses 30～100nm;
(3) at the upper evaporation First Transition layer (2) of substrate (1), on substrate, adopt electron beam evaporation to be coated with chromium rete, source parameters arranges: 300-400V, 60-100mA, rate of sedimentation 0.1-0.3nm/s, adopt the chromium particulate material that purity is 99.9%, before evaporation, carry out fritting degasification fully;
(4) being coated with of interlock adhesive linkage: selecting purity is gold or chromium or the copper film material silver-colored and that purity is 99.99wt% of 99.99wt%, adopt electron beam evaporation, and carry out abundant fritting before evaporation, affect into film quality to prevent splash, the source parameters of depositing ultrathin gold or silver layer: 300-360V, 60-90mA, rate of sedimentation 0.1-0.5nm/s, next, switch electron gun and be coated with ultra-thin chromium or copper layer, parameter setting is identical with First Transition layer; If interlock adhesive linkage is selected copper film material, need be at the upper preplating one deck copper film of First Transition layer (2), parameter setting is identical with First Transition layer, thickness 20-45nm;
(5) being coated with of metallic diaphragm: parameter setting is identical with above-mentioned ultra-thin gold or silver film, at the initial stage of evaporation process, rate of sedimentation is controlled at 0.3-0.4nm/s left and right, 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: adjusting source parameters is 80-150V, 50-70mA, changing coating process is automatic operational mode, and successively time-out is set, and adopts electron beam evaporation ZnS or Al
2o
3piece 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, on Stress match layer, replace respectively evaporation low-refraction and high-index material, thereby 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 setting is: 200-350V, 70-100mA, carries out respectively fritting fully before evaporation;
(8) being coated with of hard wear-resistant layer: setting source parameters is: 300-360V, 60-90mA, rate of sedimentation 0.1-0.5nm/s, carries out fritting degasification fully before evaporation;
(9) close ion gun and working gas and carry out in-situ annealing under 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 below 80 DEG C to substrate temperature, open vaporization chamber pickup.
7. method according to claim 6, is characterized in that: when interlock adhesive linkage is coated with, and the source parameters of depositing ultrathin gold or silver layer: 310-350V, 80-90mA, rate of sedimentation 0.2-0.4nm/s.
8. method according to claim 6, 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410369395.2A CN104090312B (en) | 2014-07-30 | 2014-07-30 | Infrared metallic reflective coating of a kind of high adhesion force and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410369395.2A CN104090312B (en) | 2014-07-30 | 2014-07-30 | Infrared metallic reflective coating of a kind of high adhesion force and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104090312A true CN104090312A (en) | 2014-10-08 |
| CN104090312B CN104090312B (en) | 2016-01-13 |
Family
ID=51638043
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410369395.2A Active CN104090312B (en) | 2014-07-30 | 2014-07-30 | Infrared metallic reflective coating of a kind of high adhesion force and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104090312B (en) |
Cited By (29)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104498887A (en) * | 2014-12-02 | 2015-04-08 | 中国航天科工集团第三研究院第八三五八研究所 | Method for preprocessing nodule defects of ultra-low-loss reflector coating substrate |
| CN104561908A (en) * | 2014-12-31 | 2015-04-29 | 西南技术物理研究所 | Preparation method for multi-waveband high-reflective film |
| CN105467619A (en) * | 2015-12-31 | 2016-04-06 | 奥特路（漳州）光学科技有限公司 | Sterilizing, anti-hard-light and wear-resisting lens and preparing method thereof |
| CN105824119A (en) * | 2016-05-19 | 2016-08-03 | 三明福特科光电有限公司 | Optical scanning galvanometer of super high reflectivity and preparation method thereof |
| CN105842758A (en) * | 2016-05-13 | 2016-08-10 | 中国科学院宁波材料技术与工程研究所 | Corrosion resistant and highly reflective front surface mirror having laminated structure and manufacture method therefor |
| CN105954824A (en) * | 2016-05-13 | 2016-09-21 | 中国科学院宁波材料技术与工程研究所 | Corrosion-resistant high-reflection front mirror and preparation method thereof |
| CN106291908A (en) * | 2016-10-18 | 2017-01-04 | 中国科学院国家天文台南京天文光学技术研究所 | Golden enhancement mode reflectance coating system and preparation method for large-scale astronomical telescope primary mirror |
| CN106435481A (en) * | 2016-10-21 | 2017-02-22 | 云南北方昆物光电科技发展有限公司 | Electrode thin-film process technology for packaging of uncooled focal plane detector |
| CN106768352A (en) * | 2016-11-25 | 2017-05-31 | 中国科学院上海技术物理研究所 | A kind of infrared narrow-band radiated source and preparation method thereof |
| CN107227460A (en) * | 2017-07-13 | 2017-10-03 | 南京波长光电科技股份有限公司 | A kind of anti-reflection DLC film by substrate of chalcogenide infrared glass and preparation method thereof |
| CN108387959A (en) * | 2018-02-28 | 2018-08-10 | 中国电器科学研究院有限公司 | A kind of high acceleration test system cold light reflector of natural light aging and its plating method |
| CN108784931A (en) * | 2018-08-19 | 2018-11-13 | 杏晖光学（厦门）有限公司 | A kind of anti-scratch hardening plating protective face mask |
| CN108977768A (en) * | 2018-09-14 | 2018-12-11 | 嘉兴岱源真空科技有限公司 | Solar heat reflecting film structure |
| CN109632630A (en) * | 2017-10-09 | 2019-04-16 | 深圳先进技术研究院 | The test method and test equipment of battery pole piece adhesive force |
| CN110441845A (en) * | 2019-07-19 | 2019-11-12 | 中国科学院上海光学精密机械研究所 | Gradational contact nano thin-layer promotes HfO2/Al2O3/SiO2The method of ultraviolet reflectance film laser damage threshold |
| CN110484869A (en) * | 2019-07-11 | 2019-11-22 | 湖北久之洋红外系统股份有限公司 | A kind of mildew resistant moistureproof optical thin film and preparation method thereof |
| CN111352180A (en) * | 2018-12-24 | 2020-06-30 | 深圳光峰科技股份有限公司 | Reflective structure, preparation method of reflective structure, and wavelength conversion device |
| CN111575656A (en) * | 2020-04-27 | 2020-08-25 | 深圳市科瀚电子有限公司 | Tuning fork oscillator and coating method thereof |
| CN112379472A (en) * | 2020-11-13 | 2021-02-19 | 上海卫星装备研究所 | Optical solar reflecting mirror with low radiation absorption ratio and preparation method thereof |
| CN112695279A (en) * | 2020-11-17 | 2021-04-23 | 威科赛乐微电子股份有限公司 | Method for plating Au by electron beam evaporation |
| CN113416933A (en) * | 2021-05-31 | 2021-09-21 | 南阳英锐光电科技有限公司 | High-reflection aluminum plating scratch-resistant coating device and coating method |
| CN113589415A (en) * | 2021-08-04 | 2021-11-02 | 南京波长光电科技股份有限公司 | Ultra-wideband YAG laser reflection film and preparation method thereof |
| CN114114490A (en) * | 2021-12-06 | 2022-03-01 | 湖北久之洋红外系统股份有限公司 | Ultralow-stress durable metal reflecting film and preparation method and application thereof |
| CN114180857A (en) * | 2021-12-16 | 2022-03-15 | 长春博信光电子有限公司 | Method for preparing silver film and substrate with silver film |
| CN114280702A (en) * | 2021-11-12 | 2022-04-05 | 福建戴斯光电有限公司 | Ultraviolet metal film layer protection process and protective layer of ultraviolet metal film |
| CN114369791A (en) * | 2021-12-24 | 2022-04-19 | 重庆四联特种装备材料有限公司 | A method for improving white spot on the surface of metal film |
| CN115185027A (en) * | 2022-06-17 | 2022-10-14 | 长春电子科技学院 | Near-infrared laser high-reflection film in space laser communication optical system and preparation method thereof |
| CN115323318A (en) * | 2022-07-07 | 2022-11-11 | 北京科技大学 | A method for improving the adhesion of diamond-based thin film resistors |
| CN119200061A (en) * | 2024-11-26 | 2024-12-27 | 武汉敢为科技有限公司 | A metal dielectric enhanced reflection film with a wavelength of 3-5µm and a preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0718250A2 (en) * | 1994-12-23 | 1996-06-26 | Saint-Gobain Vitrage | Glass substrates coated with a stack of thin layers having reflective properties for infrared and/or solar radiation |
| CN1842502A (en) * | 2003-06-26 | 2006-10-04 | 法国圣戈班玻璃厂 | Transparent substrate comprising a coating with mechanical strength properties |
| KR100860116B1 (en) * | 2008-04-18 | 2008-09-25 | 서울화학(주) | Fused Film for Glass, Manufacturing Method Thereof and Glass Fused to the Film |
| CN103412350A (en) * | 2013-08-16 | 2013-11-27 | 中国船舶重工集团公司第七一七研究所 | Multi-band enhancement type metal reflection film and preparing method thereof |
| CN103728684A (en) * | 2014-01-02 | 2014-04-16 | 杭州科汀光学技术有限公司 | High-reflectance film and manufacturing method thereof |
-
2014
- 2014-07-30 CN CN201410369395.2A patent/CN104090312B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0718250A2 (en) * | 1994-12-23 | 1996-06-26 | Saint-Gobain Vitrage | Glass substrates coated with a stack of thin layers having reflective properties for infrared and/or solar radiation |
| CN1842502A (en) * | 2003-06-26 | 2006-10-04 | 法国圣戈班玻璃厂 | Transparent substrate comprising a coating with mechanical strength properties |
| KR100860116B1 (en) * | 2008-04-18 | 2008-09-25 | 서울화학(주) | Fused Film for Glass, Manufacturing Method Thereof and Glass Fused to the Film |
| CN103412350A (en) * | 2013-08-16 | 2013-11-27 | 中国船舶重工集团公司第七一七研究所 | Multi-band enhancement type metal reflection film and preparing method thereof |
| CN103728684A (en) * | 2014-01-02 | 2014-04-16 | 杭州科汀光学技术有限公司 | High-reflectance film and manufacturing method thereof |
Cited By (42)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104498887A (en) * | 2014-12-02 | 2015-04-08 | 中国航天科工集团第三研究院第八三五八研究所 | Method for preprocessing nodule defects of ultra-low-loss reflector coating substrate |
| CN104561908A (en) * | 2014-12-31 | 2015-04-29 | 西南技术物理研究所 | Preparation method for multi-waveband high-reflective film |
| CN105467619A (en) * | 2015-12-31 | 2016-04-06 | 奥特路（漳州）光学科技有限公司 | Sterilizing, anti-hard-light and wear-resisting lens and preparing method thereof |
| CN105842758B (en) * | 2016-05-13 | 2017-11-07 | 中国科学院宁波材料技术与工程研究所 | Reflective obverse mirror of corrosion-resistant height with laminated construction and preparation method thereof |
| CN105842758A (en) * | 2016-05-13 | 2016-08-10 | 中国科学院宁波材料技术与工程研究所 | Corrosion resistant and highly reflective front surface mirror having laminated structure and manufacture method therefor |
| CN105954824A (en) * | 2016-05-13 | 2016-09-21 | 中国科学院宁波材料技术与工程研究所 | Corrosion-resistant high-reflection front mirror and preparation method thereof |
| CN105954824B (en) * | 2016-05-13 | 2017-11-07 | 中国科学院宁波材料技术与工程研究所 | Reflective obverse mirror of corrosion-resistant height and preparation method thereof |
| CN105824119A (en) * | 2016-05-19 | 2016-08-03 | 三明福特科光电有限公司 | Optical scanning galvanometer of super high reflectivity and preparation method thereof |
| CN106291908A (en) * | 2016-10-18 | 2017-01-04 | 中国科学院国家天文台南京天文光学技术研究所 | Golden enhancement mode reflectance coating system and preparation method for large-scale astronomical telescope primary mirror |
| CN106291908B (en) * | 2016-10-18 | 2021-05-11 | 中国科学院国家天文台南京天文光学技术研究所 | Gold-enhanced reflective film system for primary mirror of large astronomical telescope and preparation method |
| CN106435481A (en) * | 2016-10-21 | 2017-02-22 | 云南北方昆物光电科技发展有限公司 | Electrode thin-film process technology for packaging of uncooled focal plane detector |
| CN106435481B (en) * | 2016-10-21 | 2020-06-05 | 云南北方昆物光电科技发展有限公司 | Electrode thin film technology for packaging of uncooled focal plane detectors |
| CN106768352A (en) * | 2016-11-25 | 2017-05-31 | 中国科学院上海技术物理研究所 | A kind of infrared narrow-band radiated source and preparation method thereof |
| CN107227460B (en) * | 2017-07-13 | 2019-09-06 | 南京波长光电科技股份有限公司 | It is a kind of using chalcogenide infrared glass as anti-reflection DLC film of substrate and preparation method thereof |
| CN107227460A (en) * | 2017-07-13 | 2017-10-03 | 南京波长光电科技股份有限公司 | A kind of anti-reflection DLC film by substrate of chalcogenide infrared glass and preparation method thereof |
| CN109632630A (en) * | 2017-10-09 | 2019-04-16 | 深圳先进技术研究院 | The test method and test equipment of battery pole piece adhesive force |
| CN109632630B (en) * | 2017-10-09 | 2022-04-26 | 深圳先进技术研究院 | Test method and test equipment for battery pole piece adhesion |
| CN108387959A (en) * | 2018-02-28 | 2018-08-10 | 中国电器科学研究院有限公司 | A kind of high acceleration test system cold light reflector of natural light aging and its plating method |
| CN108784931A (en) * | 2018-08-19 | 2018-11-13 | 杏晖光学（厦门）有限公司 | A kind of anti-scratch hardening plating protective face mask |
| CN108977768A (en) * | 2018-09-14 | 2018-12-11 | 嘉兴岱源真空科技有限公司 | Solar heat reflecting film structure |
| CN111352180A (en) * | 2018-12-24 | 2020-06-30 | 深圳光峰科技股份有限公司 | Reflective structure, preparation method of reflective structure, and wavelength conversion device |
| WO2020135297A1 (en) * | 2018-12-24 | 2020-07-02 | 深圳光峰科技股份有限公司 | Reflective structure, manufacturing method of reflective structure, and wavelength conversion device |
| CN110484869A (en) * | 2019-07-11 | 2019-11-22 | 湖北久之洋红外系统股份有限公司 | A kind of mildew resistant moistureproof optical thin film and preparation method thereof |
| CN110484869B (en) * | 2019-07-11 | 2021-07-16 | 湖北久之洋红外系统股份有限公司 | Mildew-proof and damp-proof optical film and preparation method thereof |
| CN110441845A (en) * | 2019-07-19 | 2019-11-12 | 中国科学院上海光学精密机械研究所 | Gradational contact nano thin-layer promotes HfO2/Al2O3/SiO2The method of ultraviolet reflectance film laser damage threshold |
| CN111575656A (en) * | 2020-04-27 | 2020-08-25 | 深圳市科瀚电子有限公司 | Tuning fork oscillator and coating method thereof |
| CN112379472A (en) * | 2020-11-13 | 2021-02-19 | 上海卫星装备研究所 | Optical solar reflecting mirror with low radiation absorption ratio and preparation method thereof |
| CN112695279A (en) * | 2020-11-17 | 2021-04-23 | 威科赛乐微电子股份有限公司 | Method for plating Au by electron beam evaporation |
| CN113416933A (en) * | 2021-05-31 | 2021-09-21 | 南阳英锐光电科技有限公司 | High-reflection aluminum plating scratch-resistant coating device and coating method |
| CN113589415B (en) * | 2021-08-04 | 2023-03-21 | 南京波长光电科技股份有限公司 | Ultra-wideband YAG laser reflection film and preparation method thereof |
| CN113589415A (en) * | 2021-08-04 | 2021-11-02 | 南京波长光电科技股份有限公司 | Ultra-wideband YAG laser reflection film and preparation method thereof |
| CN114280702A (en) * | 2021-11-12 | 2022-04-05 | 福建戴斯光电有限公司 | Ultraviolet metal film layer protection process and protective layer of ultraviolet metal film |
| CN114280702B (en) * | 2021-11-12 | 2024-04-30 | 福建戴斯光电有限公司 | Ultraviolet metal film layer protection process and ultraviolet metal film protection layer |
| CN114114490A (en) * | 2021-12-06 | 2022-03-01 | 湖北久之洋红外系统股份有限公司 | Ultralow-stress durable metal reflecting film and preparation method and application thereof |
| CN114114490B (en) * | 2021-12-06 | 2024-07-09 | 湖北久之洋红外系统股份有限公司 | Ultralow-stress durable metal reflecting film and preparation method and application thereof |
| CN114180857A (en) * | 2021-12-16 | 2022-03-15 | 长春博信光电子有限公司 | Method for preparing silver film and substrate with silver film |
| CN114369791A (en) * | 2021-12-24 | 2022-04-19 | 重庆四联特种装备材料有限公司 | A method for improving white spot on the surface of metal film |
| CN115185027A (en) * | 2022-06-17 | 2022-10-14 | 长春电子科技学院 | Near-infrared laser high-reflection film in space laser communication optical system and preparation method thereof |
| CN115323318A (en) * | 2022-07-07 | 2022-11-11 | 北京科技大学 | A method for improving the adhesion of diamond-based thin film resistors |
| CN115323318B (en) * | 2022-07-07 | 2023-11-14 | 北京科技大学 | A method to improve the adhesion of diamond-based thin film resistors |
| CN119200061A (en) * | 2024-11-26 | 2024-12-27 | 武汉敢为科技有限公司 | A metal dielectric enhanced reflection film with a wavelength of 3-5µm and a preparation method thereof |
| CN119200061B (en) * | 2024-11-26 | 2025-02-18 | 武汉敢为科技有限公司 | Metal medium reinforced reflecting film with wavelength of 3-5 mu m and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104090312B (en) | 2016-01-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104090312B (en) | Infrared metallic reflective coating of a kind of high adhesion force and preparation method thereof | |
| TWI589448B (en) | Temperature and corrosion stable surface reflector | |
| CN105143930B (en) | It is stacked for the enhancing of high reflection mirror, durable silver coating | |
| CN103412350B (en) | Multi-band enhancement type metal reflection film and preparing method thereof | |
| EP2687875A1 (en) | Optical member and method for producing same | |
| EP1211524B9 (en) | Method for producing composition for vapor deposition, composition for vapor deposition, and method for producing optical element with antireflection film | |
| CN111679347A (en) | High damage threshold laser film process technology method | |
| WO2007013269A1 (en) | Laminated body for reflection film | |
| KR20050001425A (en) | High reflectance mirror | |
| JP2020523642A (en) | Expanding the reflection bandwidth of silver-coated laminates for high reflectors | |
| JP3387204B2 (en) | Polarizing plate, method for manufacturing polarizing plate, and liquid crystal display device | |
| WO2024093106A1 (en) | Clear-base-color, blue-light-blocking and anti-infrared resin lens and preparation method therefor | |
| CN111552012A (en) | Anti-reflection lens convenient to repair and preparation method thereof | |
| US7106515B2 (en) | Composition for vapor deposition, method for forming an antireflection film, and optical element | |
| WO2024093105A1 (en) | Weak-absorption low-reflectance clear anti-blue-light resin lens and preparation method therefor | |
| CN115421226A (en) | A kind of chalcogenide glass optical element and preparation method thereof | |
| CN101493534B (en) | Dereflection screen of display and method for making same | |
| JP2007310335A (en) | Front surface mirror | |
| JPH07104102A (en) | Water repellant reflection preventive film for glass-made optical parts and production thereof | |
| CN113817986A (en) | Coating material and preparation method thereof | |
| US20120263885A1 (en) | Method for the manufacture of a reflective layer system for back surface mirrors | |
| CN111856628A (en) | A kind of antireflection film for sapphire substrate and preparation method thereof | |
| WO2024138917A1 (en) | Weak-absorption, day/night-low-reflectance, clear-ground-color, anti-blue-light resin lens and preparation method therefor | |
| JP6627828B2 (en) | Thin film manufacturing method, thin film forming material, optical thin film, and optical member | |
| JP2020050945A (en) | Method for manufacturing optical thin film, thin film deposition material, optical thin film and optical member |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |