CN101831625A - Process for forming diamond-like carbon film on surface of infrared optical element - Google Patents
Process for forming diamond-like carbon film on surface of infrared optical element Download PDFInfo
- Publication number
- CN101831625A CN101831625A CN201010185770A CN201010185770A CN101831625A CN 101831625 A CN101831625 A CN 101831625A CN 201010185770 A CN201010185770 A CN 201010185770A CN 201010185770 A CN201010185770 A CN 201010185770A CN 101831625 A CN101831625 A CN 101831625A
- Authority
- CN
- China
- Prior art keywords
- carbon film
- diamond
- film machine
- optical element
- radio frequency
- 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.)
- Pending
Links
Landscapes
- Chemical Vapour Deposition (AREA)
Abstract
The invention relates to a process for forming a diamond-like carbon film on the surface of an infrared optical element, which is characterized by comprising the following steps: placing a monocrystalline silicon substrate in a carbon film machine, vacuumizing the carbon film machine, stopping vacuumizing the carbon film machine when the working pressure in the carbon film machine being 1.3*10-1 Pa to 1.3*10-3 Pa, filling argon in the radio-frequency source of the carbon film machine, enabling the radio-frequencyradio-frequency source of the carbon film machine to discharge to ionize the argon into the argon ions, enabling the argon ions to bombard the monocrystalline silicon substrate for 8-12 min, stopping releasing the argon, and filling the working gas of butane in the carbon film machine so that diamond-like carbon film being deposited on the surface of the infrared optical element. The diamond-like carbon film formed with the process has superior performance, corrosion resistance and high hardness.
Description
Technical field
The present invention relates to a kind of process for forming diamond-like carbon film on surface of infrared optical element.
Background technology
(Diamond-Like Carbon, DLC) research of film starts from the seventies in 20th century, mainly is the research of manufacture method in earlier stage, research manufacturing installation and the DLC membrane structure feature that adopts this device to produce to carry out quasi-diamond both at home and abroad.Recent study mainly to as if the remodeling and the technical study of producing apparatus.The DLC film at present can not large scale application subject matter comprise: the producing apparatus technical study is not enough, be difficult to large area deposition DLC film, the thin film fabrication technical study is not enough, causes thin film fabrication repeatability bad, and thin film stability and residual stress problems fundamentally do not solve.According to the basic theories of optical thin film as can be known: the DLC thin film work is when the near-infrared region; its film thickness must be greater than 400nm; when 8-12um does the infrared anti-reflection protective membrane, require film thickness usually about 1250nm, so membrane stress become the principal element that influences adhesive force.Adopt diverse ways growth DLC film, its membrane stress difference.Adopt the stress of vacuum cathode arc deposited DLC film to be approximately 4-14GPa, the stress of the DLC film of plasma enhanced chemical vapor deposition is approximately 0.18-4.7GPa, and adopting the low-priced stress of penetrating the carbon film of growth of unbalanced magnetron is 1.5-2.5GPa.With with a kind of method growth DLC film the time, the base material difference, film thickness difference, thin film fabrication technology difference, membrane stress is also different.
Summary of the invention
In order to overcome above defective, the technical problem to be solved in the present invention is: a kind of process for forming diamond-like carbon film on surface of infrared optical element is proposed, and the diamond-film-like superior performance that this technology is made, anticorrosive, the hardness height.
The technical solution adopted in the present invention is: a kind of process for forming diamond-like carbon film on surface of infrared optical element, and at first the substrate of placement silicon single crystal in carbon film machine then vacuumizes in carbon film machine, and the operating air pressure in the carbon film machine is 1.3 * 10
-1Pa--1.3 * 10
-3Stop during Pa vacuumizing, then the radio frequency source to carbon film machine charges into argon gas, radio frequency source discharge simultaneously will form argon ion after the argon gas ionization, the argon ion alignment substrate is carried out 8-12 minute bombardment, stop to discharge argon gas then, be full of the working gas butane at last in carbon film machine, promptly the monocrystalline silicon substrate surface deposition forms diamond-film-like.
According to another preferred embodiment, process for forming diamond-like carbon film on surface of infrared optical element comprises that further the working conditions of this technology is that the distance of radio frequency source and substrate is 180mm, and the flow that the gas butane charges into is 40sccm, and radio frequency power is 800w.
According to another preferred embodiment, process for forming diamond-like carbon film on surface of infrared optical element comprises that further the working conditions of this technology is that the distance of radio frequency source and substrate is between 150～250mm.
The invention has the beneficial effects as follows: the quasi-diamond film hardness height that this technology makes all do not have vestige with any sharp-pointed metal products delineation, and wear resistance is good; Raindrop diameter 2-4mm, vertical height 2m, through the 7h that drenches with rain, superficial film does not change; In humidity 95%, under the condition that temperature is 80 ℃, place 5h, rete does not have considerable change; Soak 120h in concentrated hydrochloric acid, rete does not have considerable change.
Embodiment
The present invention is further detailed explanation with preferred embodiment in conjunction with the accompanying drawings now.These accompanying drawings are the synoptic diagram of simplification, basic structure of the present invention only is described in a schematic way, so it only show the formation relevant with the present invention.
A kind of process for forming diamond-like carbon film on surface of infrared optical element, at first the substrate of placement silicon single crystal in carbon film machine then vacuumizes in carbon film machine, and the operating air pressure in the carbon film machine is 1.3 * 10
-1Pa--1.3 * 10
-3Stop during Pa vacuumizing, then the radio frequency source to carbon film machine charges into argon gas, radio frequency source discharge simultaneously will form argon ion after the argon gas ionization, the argon ion alignment substrate is carried out 8-12 minute bombardment, stop to discharge argon gas then, be full of the working gas butane at last in carbon film machine, promptly the monocrystalline silicon substrate surface deposition forms diamond-film-like.
The radio frequency source discharge is carried out ion plating and had following characteristics: 1. evaporation, ionization, three kinds of processes of acceleration can be distinguished independent control, and ionization is by RF excited; 2. 1.3 * 10
-1Pa--1.3 * 10
-3Also can stable discharging under the low operating air pressure of Pa, and the ion rate is higher; 3. carry out reactive ion plating easily; 4. compare with other ion electroplating methods, substrate temperature is controlled easily.Radio frequency source is with the working gas ionization, forms the device of ion beam current.In the deposition process of diamond-film-like, forming the needed minimum ion energy of sp3 key is 30ev, and along with the content of the increase sp3 key of ion energy also increases thereupon.In theory, when charging into the alkanes reactant gases to radio frequency source, radio frequency source just can be realized the deposition of diamond-film-like.And substrate is called target-substrate distance to ionogenic distance.
Experimental result by infrared spectral characteristic test and being analyzed as follows:
1, discharging current is to the influence of sedimentation rate
Charge into butane gas and flow to radio frequency source is 40sccm, target-substrate distance is 180mm, when radio frequency power is 800W, ionogenic discharging current is big more, the beam current density of drawing is big more, and depositing of thin film speed is high more, but when discharging current excessive, be sedimentation rate when too high, sedimentary diamond-film-like very easily comes off.
2, target-substrate distance is to the influence of sedimentation rate
Target-substrate distance not only influences the sedimentation rate of rete, and influence arrives the substrate surface energy of ions.When target-substrate distance during less than 150mm, sedimentary DLC film is easy to come off.Along with the increase of target-substrate distance, the sedimentation rate of rete descends, but the homogeneity of rete takes a favorable turn.Experiment test proves that when target-substrate distance was 250mm, film thickness uniformity (± 5%) scope can reach Φ 50mm.
3, sparking voltage is to the influence of film hardness
Ionogenic sparking voltage influences discharging current, and energy of ions is drawn in decision.And ion energy is the important parameter of decision DLC membrane structure.When ion energy is very low, be not enough to provide form the required energy of sp3 key, can only form loose sp2 bond structure; When ion energy is excessive, can impel the sp3 key to change again to sp2, form fine and close sp2 bond structure.Have only suitable ion energy could form fine and close diamond-film-like.
3, discharging current is to the influence of thin-film refractive index
For the optical property of research diamond like carbon film, thin-film refractive index is a very important parameter.When discharging current increased gradually, specific refractory power reduced gradually, increased along with the increase of discharging current subsequently.Analyze reason, this mainly is owing to the increase sparking voltage along with discharging current increases thereupon, finally cause the increase of ion energy, less in the initial stage owing to ion energy, be unfavorable for the formation of sp3 key, after discharging current was excessive, the increase of discharging current caused the increase of ion energy, thereby be beneficial to the formation of s p3 key, rete sp3 key is increased and more approaching adamantine specific refractory power.
4, silicon base 3～5 μ m actual measurement infrared spectra curve
When the thickness of twin polishing is that in 3～5 mu m ranges, peak transmittance reached more than 69 after the single face of the silicon substrate of 1mm was coated with the DLC film, average transmittances is more than 67.5%.Because the sedimentary DLC film of this method is hydrogeneous diamond-film-like, exist the stretching vibration of C2H key to absorb, make it locate to exist an absorption peak at 2325cm-1 (i.e. 4.3 μ m).The size that experiment showed, this absorption peak is not only relevant with the technology of DLC films deposited, and the kind of used working gas is relevant during also with DLC films deposited.
With above-mentioned foundation desirable embodiment of the present invention is enlightenment, and by above-mentioned description, the related work personnel can carry out various change and modification fully in the scope that does not depart from this invention technological thought.The technical scope of this invention is not limited to the content on the specification sheets, must determine its technical scope according to the claim scope.
Claims (3)
1. process for forming diamond-like carbon film on surface of infrared optical element is characterized in that: at first place the substrate of silicon single crystal in carbon film machine, then vacuumize in carbon film machine, the interior operating air pressure of carbon film machine is 1.3 * 10
-1Pa--1.3 * 10
-3Stop during Pa vacuumizing, then the radio frequency source to carbon film machine charges into argon gas, radio frequency source discharge simultaneously will form argon ion after the argon gas ionization, the argon ion alignment substrate is carried out 8-12 minute bombardment, stop to discharge argon gas then, be full of the working gas butane at last in carbon film machine, promptly the monocrystalline silicon substrate surface deposition forms diamond-film-like.
2. process for forming diamond-like carbon film on surface of infrared optical element according to claim 1 is characterized in that: the working conditions of this technology is that the distance of radio frequency source and substrate is 180mm, and the flow that the gas butane charges into is 40sccm, and radio frequency power is 800w.
3. process for forming diamond-like carbon film on surface of infrared optical element according to claim 1 is characterized in that: the working conditions of this technology is that the distance of radio frequency source and substrate is between 150～250mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010185770A CN101831625A (en) | 2010-05-28 | 2010-05-28 | Process for forming diamond-like carbon film on surface of infrared optical element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010185770A CN101831625A (en) | 2010-05-28 | 2010-05-28 | Process for forming diamond-like carbon film on surface of infrared optical element |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101831625A true CN101831625A (en) | 2010-09-15 |
Family
ID=42715844
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010185770A Pending CN101831625A (en) | 2010-05-28 | 2010-05-28 | Process for forming diamond-like carbon film on surface of infrared optical element |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101831625A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1020158C (en) * | 1987-12-22 | 1993-03-24 | 昆明物理研究所 | Method for coating diamond-like carbon film on infrared lens of germanium and silicon |
| CN1341774A (en) * | 2001-08-09 | 2002-03-27 | 中国科学院上海光学精密机械研究所 | Conductive diamond film for electrode and method for preparing the same |
| CN1557758A (en) * | 2004-02-12 | 2004-12-29 | 上海大学 | Method for making composite substrate of microstrip gas-compartment detector |
| CN1851045A (en) * | 2006-05-31 | 2006-10-25 | 大连理工大学 | Slender metal pipe inner wall diamond-film-like deposition method using DC glow discharge |
| CN101469408A (en) * | 2007-12-25 | 2009-07-01 | 中国科学院兰州化学物理研究所 | Method for depositing diamond-like carbon film on stainless steel substrate |
| CN101619455A (en) * | 2008-07-03 | 2010-01-06 | 中国科学院兰州化学物理研究所 | Super lubricating Si-doped diamond film preparation method |
-
2010
- 2010-05-28 CN CN201010185770A patent/CN101831625A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1020158C (en) * | 1987-12-22 | 1993-03-24 | 昆明物理研究所 | Method for coating diamond-like carbon film on infrared lens of germanium and silicon |
| CN1341774A (en) * | 2001-08-09 | 2002-03-27 | 中国科学院上海光学精密机械研究所 | Conductive diamond film for electrode and method for preparing the same |
| CN1557758A (en) * | 2004-02-12 | 2004-12-29 | 上海大学 | Method for making composite substrate of microstrip gas-compartment detector |
| CN1851045A (en) * | 2006-05-31 | 2006-10-25 | 大连理工大学 | Slender metal pipe inner wall diamond-film-like deposition method using DC glow discharge |
| CN101469408A (en) * | 2007-12-25 | 2009-07-01 | 中国科学院兰州化学物理研究所 | Method for depositing diamond-like carbon film on stainless steel substrate |
| CN101619455A (en) * | 2008-07-03 | 2010-01-06 | 中国科学院兰州化学物理研究所 | Super lubricating Si-doped diamond film preparation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101792895B (en) | Cathodic vacuum arc source film depositing device and method for depositing film | |
| WO2021047643A1 (en) | Reinforced nanofilm for outer cover of electronic equipment and preparation method therefor and use thereof | |
| CN105296926B (en) | A kind of anti-reflection composite membrane optical window of hard and preparation method thereof | |
| KR20120079716A (en) | Anti-fingerprint coating method and device | |
| CN107142463A (en) | A kind of plasma activated chemical vapour deposition and magnetron sputtering or the compound coating method of ion plating | |
| CN103866257B (en) | A kind of preparation method of three frequency high density plasma aid magnetron sputtering films | |
| CN201660693U (en) | Cathode vacuum arc source thin film deposition device | |
| CN105063560B (en) | The method that the AZO films that resistivity is evenly distributed are prepared using magnetron sputtering method | |
| WO2021047644A1 (en) | Electronic device, tempered reinforcement film thereof, and preparation method and application of tempered reinforcement film | |
| US7390731B2 (en) | Method of depositing an oxide layer on a substrate and a photovoltaic cell using said substrate | |
| CN104513958A (en) | Method for preparing silicon nitride film through magnetron sputtering | |
| CN105112883A (en) | Bias voltage regulation and control aperture plate plasma immersion ionic deposition DLC method | |
| CN105951051A (en) | Method of preparing graded refractive index antireflection film by adopting oblique sputtering process | |
| CN107858684B (en) | Metal-diamond-like composite coating, preparation method and application thereof and coated tool | |
| CN109576647A (en) | A kind of ultra-thin optical filter method for manufacturing thin film | |
| CN100395371C (en) | Apparatus for reinforcing arc-glow percolation plated ceating by microwave plasma and process thereof | |
| CN104480436A (en) | Method for preparing high-hardness germanium carbide film with variable refractive index | |
| CN102002683B (en) | Method for preparing hydrogen-containing diamond film | |
| CN103849847A (en) | Method of preparing diamond-like membrane by film sputtering in SiNx middle layer | |
| CN101831625A (en) | Process for forming diamond-like carbon film on surface of infrared optical element | |
| CN101736313B (en) | Method for preparing diamond-like film on germanium substrate | |
| CN108220897A (en) | The method of magnetron sputtering low temperature preparation vanadium dioxide film | |
| CN102041552A (en) | Method for preparing polysilicon membrane | |
| CN115029669B (en) | Method for improving deposition efficiency by adopting liquid metal high-power pulse magnetron sputtering | |
| CN109837522A (en) | A kind of forming diamond-like carbon film on surface of infrared optical element coating process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Gu Hua Inventor after: Chen Guoqing Inventor before: Gu Hua Inventor before: Chen Guoqing Inventor before: Li Shuang |
|
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100915 |