CN103287010B - Sapphire infrared window yittrium oxide/silica anti-reflection protective film and preparation method thereof - Google Patents
Sapphire infrared window yittrium oxide/silica anti-reflection protective film and preparation method thereof Download PDFInfo
- Publication number
- CN103287010B CN103287010B CN201310031456.XA CN201310031456A CN103287010B CN 103287010 B CN103287010 B CN 103287010B CN 201310031456 A CN201310031456 A CN 201310031456A CN 103287010 B CN103287010 B CN 103287010B
- Authority
- CN
- China
- Prior art keywords
- sapphire
- protective film
- infrared window
- argon gas
- sio
- 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.)
- Active
Links
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
The invention provides a kind of sapphire infrared window yittrium oxide/silica anti-reflection protective film, comprise the yttrium oxide layer and silicon dioxide layer that deposit successively, the thickness of described yttrium oxide layer is 200 ~ 750nm, and the thickness of described silicon dioxide layer is 600 ~ 900nm.Sapphire infrared window yittrium oxide/silica anti-reflection protective film provided by the invention; while raising sapphire elevated temperature strength and infrared wave transmission rate; especially can improve the adhesion property of anti-reflection protective film, thus solve Thermal cracking, thermal distoftion and diaphragm that sapphire infrared window often occurs at the harsh environments such as high temperature, high pressure and the problem such as to come off.
Description
Technical field
The present invention relates to thin film technique field, particularly relate to a kind of sapphire infrared window yittrium oxide/silica anti-reflection protective film and preparation method thereof.
Background technology
Infrared sensing/imaging system and outside adverse circumstances, as the important component part of infrared imaging detection system, are mainly separated by infrared window.For infrared window, infrared sensor and other electrooptical device should be protected on the one hand not by the damage of external environment, ensure again can not reduce photoelectric sensor to the detectivity of transmitted spectrum signal and resolution ratio simultaneously.
Sapphire crystal, owing to having the combination properties such as good machinery and optics, is the main candidate material of medium wave (3 ~ 5 μm) infrared window.But, along with the development of aircraft high speed trend, higher technological challenge is proposed to infrared acquisition window: serious Aerodynamic Heating, sapphire infrared window operating temperature will be caused also constantly to increase thereupon, adverse influence can be brought to mechanical performances such as the strength and stiffness of sapphire infrared window device, greatly reduce the wave penetrate capability that it is good in addition, thus produce the serious problems such as such as Thermal cracking, heat radiation and light distortion, cause the structure/disabler of sapphire infrared window parts.Under the harsh environments such as high temperature, high pressure, the intensity of sapphire infrared window material and transmitance also can significantly decline, and will produce the phenomenons such as Thermal cracking, heat radiation and light distortion thereupon, thus cause the structure/disabler of infrared window parts.
At present, both at home and abroad for improving the method for sapphire infrared window higher device temperature intensity, being all based on minimizing blemish, stoping twin formation and improve the aspects such as stress state; And for affecting the factor of sapphire high temperature wave transmission rate, reduce its high temperature emissive rate, main or prepare corresponding anti-reflection film by appropriate design.Therefore, have the main modified measures of sapphire infrared window: heat treatment, doping solution strengthening, precipitation strength, ion implantation and surface coating etc.
Plated surface embrane method refers at sapphire surface formation compression rete, to reduce flaw size and to strengthen the stress needed for Crack Extension, thus stops Defect expanding, improves the intensity of material.The selection of superficial film composition, the thermal coefficient of expansion that should meet film lower than sapphire, to ensure that sapphire surface is in compressive stress state; Simultaneously in order to meet high load bearing requirements, good interface cohesion must can be realized between rete and sapphire, to ensure higher adhesive force.
Air-sea tactical operations center of the U.S. adopts radio-frequency magnetron sputter method to prepare individual layer SiO on a sapphire substrate
2film and three layers of SiO
2/ Si
3n
4/ SiO
2laminated film, to improve sapphire infrared transmittivity and elevated temperature strength.But, due to SiO
2the thermal coefficient of expansion of film and Sapphire Substrate has big difference, and causes producing larger thermal stress when temperature is undergone mutation, and this thermal stress can reduce the adhesive force between film and substrate greatly, even can have influence on the heat endurance of whole window.
In addition, Northwestern Polytechnical University and Taiwan National Central University also once adopted silicon nitride film as transition zone, at sapphire surface sputtering SiO
2/ Si
3n
4double shielding film.But because the content of the usual nitrogen of silicon nitride of sputtering is on the low side, more difficultly meet stoichiometric proportion, the Components Chemical formula of film is SiN
xo
y; The effect of adhesion property and anti-reflection protection is all not ideal enough, needs to be further improved.
Summary of the invention
For solve problems of the prior art, inventor using Yttrium oxide thin film as sapphire infrared window SiO
2the growth intermediate layer of diaphragm, can alleviate sapphire and SiO
2thermal mismatch problem between film: pass through Y
2o
3layer and SiO
2the deposition successively of layer, can improve Y
2o
3/ SiO
2the stress state of anti-reflection protective film and adhesion property, improve the tensile strength of film-substrate interface, thus the elevated temperature strength of enhancing sapphire infrared window, high temperature wave penetrate capability and anti-quenching thermal shock ability.
An aspect, the invention provides a kind of sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film, comprises the Y deposited successively
2o
3layer and SiO
2layer, described Y
2o
3the thickness of layer is 200 ~ 750nm, described SiO
2the thickness of layer is 600 ~ 900nm.
Adopt technique scheme, sapphire infrared window Y provided by the invention
2o
3/ SiO
2anti-reflection protective film is while raising sapphire elevated temperature strength and infrared wave transmission rate; especially can improve the adhesion property of anti-reflection protective film, thus solve Thermal cracking, thermal distoftion and diaphragm that sapphire infrared window often occurs at the harsh environments such as high temperature, high pressure and the problem such as to come off.
Sapphire crystal itself cannot meet the requirement such as high strength and high wave transmission rate to infrared window under harsh environments.Existing silicon oxide film is used as sapphire anti-reflection protective film, while raising sapphire infrared window intensity, can improve its infrared wave transmission rate, but there is the problem of thermal mismatching between silicon oxide film and sapphire.When temperature is more than 200 DEG C, yittrium oxide (Y
2o
3) the film thermal coefficient of expansion is less than sapphire thermal coefficient of expansion, using Yttrium oxide thin film as sapphire infrared window SiO
2diaphragm growth intermediate layer, when at high temperature using, can alleviate sapphire and SiO
2thermal mismatch problem between film.And yittrium oxide in the event of high temperatures, can keep tiny oxide, these oxides make crystal boundary be strengthened by hindering the factor such as dislocation motion and stable dislocation substructure, thus ensure that it has good high-temperature mechanical property.The existence in Yttrium oxide thin film intermediate layer, will improve Y
2o
3/ SiO
2the stress state of anti-reflection protective film, improves the tensile strength of film-substrate interface, is conducive to improving Y
2o
3/ SiO
2the adhesion property of anti-reflection protective film.In addition, yittrium oxide is a kind of well infrared optical material, has the advantage of high permeability, low-launch-rate in middle-infrared band, and the refractive index of yittrium oxide higher (during λ=3.75 μm, n=1.86).The present invention is by Y
2o
3the SiO of film and low-refraction
2the duplicature that film (during λ=3.75 μm, n=1.39) forms, can have good infrared anti-reflection effect to sapphire (during λ=3.75 μm, n=1.69), thus improves the infrared wave transmission rate of sapphire infrared window.
As a further improvement on the present invention, described Y
2o
3the thickness of layer is 350 ~ 600nm, described SiO
2the thickness of layer is 700 ~ 800nm.
As a further improvement on the present invention, described Y
2o
3the thickness of layer is 500nm, described SiO
2the thickness of layer is 700nm.
On the other hand, the present invention also provides sapphire infrared window Y
2o
3/ SiO
2the preparation method of anti-reflection protective film, comprises the steps:
A) Sapphire Substrate is placed on the sample substrate platform of magnetron sputtering chamber, vacuum chamber is vacuumized, behind heated substrate sample stage to 300 ~ 500 DEG C, argon gas is passed into again to chamber, and open radio-frequency power supply, metallic yttrium target is applied to the sputtering power starter of 100 ~ 250W, carry out pre-sputtering, to remove the oxide layer of metallic yttrium target material surface;
B) pass into argon gas and oxygen after pre-sputtering simultaneously, and open matrix baffle plate, surface coating is carried out to Sapphire Substrate, deposit after 150 ~ 600 minutes, form Y
2o
3layer, closes substrate baffle plate, closes radio-frequency power supply and argon gas source;
C) rotary sample chip bench, makes Sapphire Substrate downwards just to corresponding silicon target, again passes into argon gas, and open radio-frequency power supply to vacuum chamber, silicon target is applied to the sputtering power starter of 100 ~ 250W, carry out pre-sputtering, to remove the oxide layer on silicon target surface;
D) pass into argon gas and oxygen after pre-sputtering simultaneously, open matrix baffle plate, again surface coating is carried out to Sapphire Substrate, deposit after 60 ~ 90 minutes, form SiO
2skin, thus obtained sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film.
Adopt technique scheme, the sapphire infrared window Y of preparation
2o
3/ SiO
2anti-reflection protective film, has good stress state and adhesion property, can improve the elevated temperature strength of sapphire infrared window, high temperature wave penetrate capability and anti-quenching thermal shock ability.
As a further improvement on the present invention, the vacuum vacuumized described in is 4.0 × 10
-4~ 2.0 × 10
-4pa.
As a further improvement on the present invention, in described steps A and step C, the flow-control of argon gas is at 10 ~ 50mL/min, and chamber inner pressure is by force 3 ~ 5Pa.
As a further improvement on the present invention, in described step B, the flow-control of argon gas is at 10 ~ 50mL/min, and the flow of oxygen is 10 ~ 20mL/min, and the pressure in chamber is 5 ~ 15Pa.
As a further improvement on the present invention, in described step D, the flow-control of argon gas is at 10 ~ 50mL/min, and the flow of oxygen is 10 ~ 20mL/min, and the pressure in chamber is 0.5 ~ 2Pa.
As a further improvement on the present invention, preparation method provided by the invention also comprises step: E) by described sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film is closing baffle plate, radio-frequency power supply and argon gas source after sputtering, and oxygen atmosphere situ insulation 60 ~ 120 minutes.After sputtering obtains anti-reflection protective film, lead to oxygen thermal insulation a period of time in chamber original position, sputtering state Y can be improved
2o
3/ SiO
2the non-chemical proportion anoxia phenomenon of anti-reflection protective film, improves Y
2o
3/ SiO
2the hardness of anti-reflection protective film, makes Y simultaneously
2o
3/ SiO
2the actual refractive index of anti-reflection protective film, close to the refractive index of theory, plays better anti-reflection protected effect.
Compared with prior art, the invention has the beneficial effects as follows: sapphire infrared window Y provided by the invention
2o
3/ SiO
2anti-reflection protective film, while raising sapphire infrared window elevated temperature strength and infrared wave transmission rate, especially can improve sapphire infrared window Y
2o
3/ SiO
2the adhesion property of anti-reflection protective film, thus solve Thermal cracking, thermal distoftion and diaphragm that sapphire infrared window often occurs at the harsh environments such as high temperature, high pressure and the problem such as to come off.Sapphire infrared window Y provided by the invention
2o
3/ SiO
2anti-reflection protective film can improve the tensile strength of film-substrate interface, thus the elevated temperature strength of enhancing sapphire infrared window, high temperature wave penetrate capability and anti-quenching thermal shock ability, realize the multi-field extensive use of sapphire infrared window.Preparation method provided by the invention is simple, obtained sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film has good stress state and adhesion property, can improve the elevated temperature strength of sapphire infrared window, high temperature wave penetrate capability and heat-resistant impact ability.
Accompanying drawing explanation
Fig. 1 is sapphire infrared window Y
2o
3/ SiO
2the SEM cross-section morphology of anti-reflection protective film.
Fig. 2 is sapphire surface 350nmY
2o
3/ 670nmSiO
2the nanometer cut resolution chart of duplicature; Wherein, 2-a) be scratch depth-displacement curve, 2-b) be cut optical microphotograph pattern.
Fig. 3 is sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film has different-thickness Y
2o
3critical load schematic diagram during intermediate layer.
Fig. 4 is the surface topography before and after sapphire plated film after 225 DEG C of thermal shocks three times; Wherein, 4-a) be non-plated film sapphire, 4-b) be the thick SiO of sapphire two-sided plating 670nm
2film, 4-c) be the two-sided plating 500nmY of sapphire
2o
3/ 670nmSiO
2duplicature.
Fig. 5 is sapphire and two-sided plating Y thereof
2o
3/ SiO
2the average wave transmission rate schematic diagram of alternating temperature after anti-reflection protective film.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further details.
embodiment one sapphire infrared window Y
2
o
3
/ SiO
2
anti-reflection protective film.
Sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film, comprises the Y deposited successively
2o
3layer and SiO
2layer, Y
2o
3the thickness of layer is 500nm, SiO
2the thickness of layer is 700nm.Sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film is with Y
2o
3layer is growth intermediate layer, can improve the tensile strength of film-substrate interface, thus the elevated temperature strength of enhancing sapphire infrared window, high temperature wave penetrate capability and anti-quenching thermal shock ability, realize the multi-field extensive use of sapphire infrared window.
embodiment two sapphire infrared window Y
2
o
3
/ SiO
2
anti-reflection protective film.
Sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film, comprises the Y deposited successively
2o
3layer and SiO
2layer, Y
2o
3the thickness of layer is 350nm, SiO
2the thickness of layer is 800nm.Sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film is with Y
2o
3layer is growth intermediate layer, can improve the tensile strength of film-substrate interface, thus the elevated temperature strength of enhancing sapphire infrared window, high temperature wave penetrate capability and anti-quenching thermal shock ability, realize the multi-field extensive use of sapphire infrared window.
embodiment three sapphire infrared window Y
2
o
3
/ SiO
2
the preparation of anti-reflection protective film.
First, get silicon and metallic yttrium target, remove the oxide layer of silicon and metallic yttrium target material surface with sand papering, after ethanol purge 15 ~ 30min, be placed on two radio frequency target position corresponding to magnetron sputtering chamber respectively; Then, Sapphire Substrate is placed on the sample substrate platform of magnetron sputtering chamber, vacuum is evacuated to vacuum chamber and reaches 2.0 × 10
-4pa, heated substrate sample stage to 350 DEG C, argon gas is passed into vacuum chamber, the flow-control of argon gas is at 20mL/min, when chamber inner pressure is by force 3 ~ 5Pa, open radio-frequency power supply, metallic yttrium target is applied to the sputtering power starter of 100 ~ 250W, pre-sputtering 10 minutes, so that the oxide layer removing metallic yttrium target material surface further; Then, while logical argon gas, pass into oxygen, wherein the flow of oxygen is 10mL/min, when the pressure in chamber is 5 ~ 15Pa, opens substrate baffle plate, carries out surface coating to Sapphire Substrate, deposits after 400 minutes, forms Y
2o
3layer, closes substrate baffle plate, closes radio-frequency power supply and argon gas source.
Rotary sample chip bench, make Sapphire Substrate downwards just to corresponding silicon target, and again pass into argon gas to vacuum chamber, wherein the flow-control of argon gas is at 20mL/min.When chamber inner pressure is by force 3 ~ 5Pa, open radio-frequency power supply, silicon target is applied to the sputtering power starter of 100 ~ 250W, carry out pre-sputtering 10 minutes, to remove the oxide layer on silicon target surface further.Then, while logical argon gas, again pass into oxygen, wherein the flow of oxygen is 10mL/min.When the pressure in chamber is 0.5 ~ 2Pa, open substrate baffle plate, again surface coating is carried out to Sapphire Substrate, deposit after 80 minutes, form SiO
2layer, obtained sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film.
By obtained sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film, with its cross-section morphology of scanning electron microscope test, result as shown in Figure 1.As can be seen from Figure 1, define at sapphire surface with Y
2o
3for internal layer, SiO
2for outer field anti-reflection protective film; Film thickness is uniformity comparatively, and has no obvious obscission, illustrates that film base combines good.
embodiment four sapphire infrared window Y
2
o
3
/ SiO
2
the preparation of anti-reflection protective film.
First, get silicon and metallic yttrium target, remove the oxide layer of silicon and metallic yttrium target material surface with sand papering, after ethanol purge 15 ~ 30min, be placed on two radio frequency target position corresponding to magnetron sputtering chamber respectively; Then, Sapphire Substrate is placed on the sample substrate platform of magnetron sputtering chamber, vacuum is evacuated to vacuum chamber and reaches 4.0 × 10
-4pa, heated substrate sample stage to 500 DEG C, passes into argon gas to vacuum chamber, and the flow-control of argon gas is at 50mL/min.When chamber inner pressure is by force 3 ~ 5Pa, open radio-frequency power supply, metallic yttrium target is applied to the sputtering power starter of 100 ~ 250W, carry out pre-sputtering 10 minutes, to remove the oxide layer of metallic yttrium target material surface further.Then, while logical argon gas, then pass into oxygen, wherein the flow of oxygen is 20mL/min.When the pressure in chamber is 5 ~ 15Pa, open matrix baffle plate, surface coating is carried out to Sapphire Substrate, deposit after 600 minutes, form Y
2o
3layer, closes substrate baffle plate, closes radio-frequency power supply and argon gas source.
Rotary sample chip bench, make Sapphire Substrate downwards just to corresponding silicon target, and again pass into argon gas to vacuum chamber, wherein the flow-control of argon gas is at 50mL/min.When the pressure in chamber is 3 ~ 5Pa, open radio-frequency power supply, silicon target is applied to the sputtering power starter of 100 ~ 250W, carry out pre-sputtering 10 minutes, to remove the oxide layer on silicon target surface further; Then, while logical argon gas, then pass into oxygen, wherein the flow of oxygen is 20mL/min.When the pressure in chamber is 0.5 ~ 2Pa, open substrate baffle plate, again surface coating is carried out to Sapphire Substrate; Deposit after 90 minutes, form SiO
2layer, obtained sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film.
embodiment five sapphire infrared window Y
2
o
3
/ SiO
2
the effect example of anti-reflection protective film.
To sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film carries out cut test, and result of the test as shown in Figure 2.As can be seen from Fig. 2-a), to 350nmY
2o
3/ 670nmSiO
2duplicature, carving the incipient stage (0 ~ 364nm) of scan depths-displacement curve, along with forward load linearly increases, scratch depth also approximately linear increases, but there is no catastrophe point, this shows that film increases with load in this course and there is no generation peeling phenomenon.Horizontal displacement is at 364nm place, and load is increased to certain value, and putting the degree of depth under obviously increases suddenly, and this shows that film starts to break or peel off, and now corresponding load is called that loading critical value (is denoted as Lc
l).The horizontal displacement (286nm) that then scan depths-displacement curve catastrophe point is corresponding, less than the horizontal displacement (364nm) loaded corresponding to critical value, and film now peels off, as Fig. 2-b) shown in.And the region of horizontal displacement between 286 ~ 364nm, carving scan depths-displacement curve linearly increases along with load and increases, and obviously fluctuation occurs then scan depths-displacement curve.This phenomenon shows in scratching process, and film plastic deformation occurs along with load increases but does not peel off; But after unloading, film peels off: this is mainly flexible film-hard substrate due to sample, and in scratching process, film bears more plastic deformation; And after unloading, what film and substrate elastic deformation recovered asynchronously causes film separation.Load corresponding to rear scan depths-displacement curve catastrophe point is called that unloading critical value (is denoted as Lc
u).
Fig. 3 is that film has different-thickness Y
2o
3critical load schematic diagram during intermediate layer.As can be seen from Figure 3, Y is worked as
2o
3layer thickness when 200 ~ 650nm scope, sapphire infrared window Y
2o
3/ SiO
2the critical load of anti-reflection protective film is all higher; Especially Y
2o
3when the thickness of layer is 500nm, critical load reaches 50mN.But work as Y
2o
3layer thickness more than after 500nm, along with Y
2o
3the increase of layer thickness, critical load reduces on the contrary.
For evaluating the thermal shock resistance of film, plated film and non-plated film sapphire are heated up respectively, then the water put under room temperature carries out quenching chilling.The test of quenching thermal shock shows, quenching when non-plated film sapphire is heated to 200 DEG C just occurs macroscopic cracking, and two-sided plating Y
2o
3/ SiO
2there is the heating-up temperature that macroscopic cracking is corresponding in the sapphire quenching of duplicature, is then 225 DEG C.By non-plated film sapphire, two-sided plating SiO
2film sapphire and two-sided plating Y
2o
3/ SiO
2the sapphire samples of duplicature is heated to 225 DEG C respectively, then carries out water hardening.After quenching cycles three times, the surperficial macroscopic cracking (as shown in Figure 4) of comparative sample.As can be seen from Figure 4, two-sided plating Y
2o
3/ SiO
2the macroscopic cracking of duplicature sapphire surface is less, shows best thermal shock resistance.
In addition, for investigating sapphire infrared window Y
2o
3/ SiO
2the high temperature wave penetrate capability of anti-reflection protective film, to the non-plated film of sapphire and two-sided plating SiO thereof
2diaphragm, Y
2o
3/ SiO
2the average wave transmission rate of alternating temperature after anti-reflection protective film carries out detecting and comparing, and result as shown in Figure 5.As can be seen from Figure 5, the average wave transmission rate before and after sapphire plated film all declines along with the rising of temperature, but the amplitude declined along with the rising of temperature during the non-plated film of sapphire is larger; And the thick SiO of two-sided plating 670nm
2diaphragm, 350nmY
2o
3/ 670nmSiO
2anti-reflection protective film and 500nmY
2o
3/ 670nmSiO
2the sapphire samples of anti-reflection protective film, the amplitude declined along with the rising of temperature is less, is all much higher than wave transmission rate during the non-plated film of sapphire.
Therefore compared to SiO
2monofilm, introduces Y
2o
3intermediate layer, the Y of preparation
2o
3/ SiO
2film, while raising sapphire infrared window thermal shock resistance, can not reduce sapphire infrared window antireflective effect; It is a kind of sapphire infrared window anti-reflection protective film having applications well prospect.
Above content is in conjunction with concrete preferred embodiment further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (1)
1. a preparation method for sapphire infrared window yittrium oxide/silica anti-reflection protective film, is characterized in that:
Described sapphire infrared window yittrium oxide/silica anti-reflection protective film comprises the yttrium oxide layer and silicon dioxide layer that deposit successively, and the thickness of described yttrium oxide layer is 200 ~ 750nm, and the thickness of described silicon dioxide layer is 600 ~ 900nm;
Described method comprises the steps:
A) Sapphire Substrate is placed on the sample substrate platform of magnetron sputtering chamber, vacuum chamber is vacuumized, heated sample chip bench to 300 ~ 500 DEG C, argon gas is passed into again to chamber, and open radio-frequency power supply, metallic yttrium target is applied to the sputtering power starter of 100 ~ 250W, carry out pre-sputtering, to remove the oxide layer of metallic yttrium target material surface;
B) pass into argon gas and oxygen after pre-sputtering simultaneously, and open substrate baffle plate, surface coating is carried out to Sapphire Substrate, deposit after 150 ~ 600 minutes, form Y
2o
3layer, closes substrate baffle plate, closes radio-frequency power supply and argon gas source;
C) rotary sample chip bench, makes Sapphire Substrate downwards just to corresponding silicon target, again passes into argon gas to vacuum chamber, and open radio-frequency power supply, silicon target is applied to the sputtering power starter of 100 ~ 250W, carry out pre-sputtering, to remove the oxide layer on silicon target surface;
D) pass into argon gas and oxygen after pre-sputtering simultaneously, open substrate baffle plate, again surface coating is carried out to Sapphire Substrate, deposit after 60 ~ 90 minutes, form SiO
2skin, thus obtained sapphire infrared window Y
2o
3/ SiO
2anti-reflection protective film;
E) described sapphire infrared window yittrium oxide/silica anti-reflection protective film is closed substrate baffle plate, radio-frequency power supply and argon gas source after sputtering, oxygen atmosphere situ insulation 60 ~ 120 minutes;
In described steps A and step C, the flow-control of argon gas is at 10 ~ 50mL/min, and chamber inner pressure is by force 3 ~ 5Pa;
In described step B, the flow-control of argon gas is at 10 ~ 50mL/min, and the flow of oxygen is 10 ~ 20mL/min, and the pressure in chamber is 5 ~ 15Pa.
In described step D, the flow-control of argon gas is at 10 ~ 50mL/min, and the flow of oxygen is 10 ~ 20mL/min, and the pressure in chamber is 0.5 ~ 2Pa;
The described vacuum vacuumized is 4.0 × 10
-4~ 2.0 × 10
-4pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310031456.XA CN103287010B (en) | 2013-01-28 | 2013-01-28 | Sapphire infrared window yittrium oxide/silica anti-reflection protective film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310031456.XA CN103287010B (en) | 2013-01-28 | 2013-01-28 | Sapphire infrared window yittrium oxide/silica anti-reflection protective film and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103287010A CN103287010A (en) | 2013-09-11 |
| CN103287010B true CN103287010B (en) | 2016-04-13 |
Family
ID=49088779
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310031456.XA Active CN103287010B (en) | 2013-01-28 | 2013-01-28 | Sapphire infrared window yittrium oxide/silica anti-reflection protective film and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103287010B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105821387B (en) * | 2016-04-05 | 2018-08-17 | 南京航空航天大学 | Sapphire optical performance improvement method based on micron order array structure and Yttrium oxide thin film |
| JP7189371B2 (en) * | 2019-09-30 | 2022-12-13 | 京セラ株式会社 | Member for plasma processing apparatus and plasma processing apparatus provided with the same |
| KR20240035883A (en) * | 2021-08-31 | 2024-03-18 | 교세라 가부시키가이샤 | Plasma-resistant laminate, manufacturing method thereof, and plasma processing device |
| CN114196927B (en) * | 2021-11-25 | 2024-02-27 | 深圳先进技术研究院 | Ultraviolet anti-reflection glass based on sapphire substrate and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050201422A1 (en) * | 2004-02-16 | 2005-09-15 | Tatsuo Ohta | Optical element and optical pickup apparatus |
| CN101368263A (en) * | 2008-09-28 | 2009-02-18 | 西北工业大学 | Preparation method of silicon nitride/silicon oxide double-layer anti-reflection protective film |
-
2013
- 2013-01-28 CN CN201310031456.XA patent/CN103287010B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050201422A1 (en) * | 2004-02-16 | 2005-09-15 | Tatsuo Ohta | Optical element and optical pickup apparatus |
| CN101368263A (en) * | 2008-09-28 | 2009-02-18 | 西北工业大学 | Preparation method of silicon nitride/silicon oxide double-layer anti-reflection protective film |
Non-Patent Citations (2)
| Title |
|---|
| 红外窗口用二氧化硅/氧化钇增透膜的优化制备与评价;李云刚;《中国优秀硕士学位论文全文数据库工程科技I辑》;20110615(第06期);第14页2.2节，第15页2.3节，第28页4.1节 * |
| 红外窗口用蓝宝石晶体Y2O3/SiO2增透薄膜的设计与制备研究;吴智雄;《中国优秀硕士学位论文全文数据库基础学科辑》;20111215(第S2期);第36页3.2节，第37页3.3节，40页4.1节 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103287010A (en) | 2013-09-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103287010B (en) | Sapphire infrared window yittrium oxide/silica anti-reflection protective film and preparation method thereof | |
| WO2018188154A1 (en) | Structure of full-solid-state thin-film electrochromic device and preparation method therefor | |
| CN106526719B (en) | Homogeneity bilayer SiO2The automatically cleaning antireflective film compound with polytetrafluoroethylene (PTFE) and preparation method | |
| CN111158069B (en) | Spectrum selective radiation infrared stealth material and preparation method thereof | |
| JP2009510263A (en) | Sputtering target, low resistance transparent conductive coating, method for forming such coating and composition for use in the conductive coating | |
| CN104775101A (en) | Preparation method and application of porous vanadium dioxide thin film | |
| CN102251216A (en) | Method for preparing tungsten-doped vanadium oxide film | |
| CN103770403A (en) | Heat-reflective coated glass capable of being tempered | |
| CN102219396A (en) | Temperable gold low-emissivity coated glass and manufacturing method thereof | |
| CN104393061B (en) | A kind of crystal silicon solar energy battery antireflective coating and preparation technology thereof | |
| CN103981500B (en) | A kind of surface micro-structure improving vanadium dioxide film phase time-varying amplitude | |
| CN108220897B (en) | The method of magnetron sputtering low temperature preparation vanadium dioxide film | |
| CN101159178A (en) | Transparency conductive film and preparation method thereof | |
| CN112410734A (en) | Medium-wave infrared transparent electromagnetic shielding film and preparation method thereof | |
| Bingyan et al. | Preparation and characteristics of indium tin oxide (ITO) thin films at low temperature by rf magnetron sputtering | |
| CN109554660B (en) | Preparation method of high-entropy alloy surface boronizing layer | |
| CN109182969B (en) | Preparation method of medium-wave infrared optical hard protective film | |
| Liu et al. | Effect of Sputtering Power on Nano-mechanical Properties of SiCO Film | |
| KR102399299B1 (en) | Center Lift Pin for Chemical Vapor Deposition | |
| CN110846615B (en) | Micro-nano structure layer and method for improving binding force of fluorinated diamond-like carbon film and steel substrate | |
| CN109182974A (en) | A method of vanadium oxide film is prepared by two one-step rapid thermal anneals | |
| CN102650044B (en) | A kind of preparation method of SGZO-Au-SGZO nesa coating | |
| CN109468604B (en) | Preparation method of high-transmittance IGZO (indium gallium zinc oxide) thin film | |
| Gu et al. | Preparation, structure and optical properties of transparent conducting gallium-doped zinc oxide thin films | |
| Jing et al. | Investigation of the effects of AR layers on the structure and properties of transparent conductive oxide thin films |
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 |