CN101550541A - Linear ion beam source apparatus and method for depositing diamond like carbon (DLC) film by the apparatus - Google Patents
Linear ion beam source apparatus and method for depositing diamond like carbon (DLC) film by the apparatus Download PDFInfo
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- CN101550541A CN101550541A CNA2009100987101A CN200910098710A CN101550541A CN 101550541 A CN101550541 A CN 101550541A CN A2009100987101 A CNA2009100987101 A CN A2009100987101A CN 200910098710 A CN200910098710 A CN 200910098710A CN 101550541 A CN101550541 A CN 101550541A
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Abstract
The invention relates to a linear ion beam source apparatus and a method for depositing diamond like carbon (DLC) film by the apparatus. The apparatus includes: a cathode (1), a anode (2), an ionization area (7) formed between the the cathode (1) and the anode (2), a gas supplying channel (4) for guiding the ionogenic gas into the ionization area (7), and a magnet (3) for generating magnetic field distribution in the ionization area (7). The invention is characterized in that: a circular slit (13) is formed on the cathode (1) to divide the cathode (1) into a first cathode (11) in the circular slit (13) and a second cathode (12) out of the circular slit (13); while the anode (2) is also in circular structure, and is displaced on the position relative to the circular slit (13) of the cathode (1). Compared with the current technologies, The apparatus provided in the invention can generate continuous homogeneous ion beam stream in larger size range; the film prepared by the method in the invention achieves the advantages of high hardness, good film/base adhesion, smooth surface, low friction coefficient and even thickness.
Description
Technical field
The present invention relates to a kind of linear ion beam source apparatus and utilize the method for this device depositing diamond-like carbon film.
Background technology
Quasi-diamond (Diamond-like carbon, DLC) film is because of having high rigidity, low-friction coefficient, good corrosion-proof wear, particular performances such as wide transparency range and splendid bioaffinity are widely used in industrial production such as instrument, mould, automobile, magnetic storage, microelectronics and the real daily life.Especially ultra-low friction coefficient that under the extreme operating condition condition, shows because of it and good friction durability, having demonstrated good prospects for application in high-tech sectors such as Aeronautics and Astronautics, is one of the research focus of novel in recent years carbon functional materials and tribological field and important branch.
At present, the deposition technique of diamond like carbon film mainly contain physical vaporous deposition (Physical Vapor Deposition, PVD), chemical vapour deposition technique (Chemical Vapor Deposition, CVD) and liquid phase electrochemical deposition method three major types.Physical vaporous deposition mainly comprises the ion beam depositing that utilizes carbon-source gas and utilizes methods such as the magnetron sputtering of solid graphite target, cathodic vacuum arc deposition; Chemical Vapor deposition process mainly contains plasma enhanced CVD, heated filament CVD and microwave plasma cyclotron resonance CVD etc.Compare the PVD method, this method depositing temperature is higher, be difficult to realize deposition on thermally sensitive base materials such as plastics, and film-substrate cohesion is generally relatively poor; The liquid phase electrochemical deposition method is a kind of novel wet type synthetic method of rising in recent years, mainly prepare diamond-film-like by electrolysis organic solution, equipment is simple though this method has, the advantage of mild condition, but synthetic thin film physics, chemical property and technology stability are relatively poor, and existing many places are in the experimental exploring stage.Comprehensive, the PVD method is synthetic at present diamond-like carbon film common used in industry technology, but because of all there are following problems in these methods, has seriously restricted the widespread use of diamond-like carbon film:
The DLC carbon film that tradition heated filament ion beam is prepared has little, the ganoid advantage of unrelieved stress, but the long-time use of heated filament causes the reduction of plasma body ionization level, quality of forming film variation easily on the one hand, designed by most of ionogenic cylindrical structurals, the even area of film of this method growth is less, be difficult to realize the big area Industry Promotion, but though a plurality of ionogenic parallel use enlarged-area, the corresponding raising of cost with the equipment complexity;
Depositing temperature is low though magnetron sputtering DLC thin film technique has, large area deposition easily, the characteristics of technology maturation, film growth rate is lower, film-substrate cohesion, be difficult to deposition on base materials such as metal, easily spalling failure;
Cathodic vacuum arc DLC carbon film has sedimentation rate height, ion energy is big, film-substrate cohesion is good advantage, but because of the existence of electric arc melting arc spot often causes film surface to deposit a large amount of macroscopical macrobeads, surface irregularity, degradation, though add to a certain degree head it off of magnetic filter, but therefore depositing of thin film speed can decline to a great extent, and the relevant device complex and expensive.
Summary of the invention
First technical problem to be solved by this invention is to provide a kind of linear ion beam source apparatus that can produce continuous uniform ion line in larger size range, be beneficial to the big area uniform deposition at above-mentioned prior art.
Second technical problem to be solved by this invention provides a kind of method for preparing the even diamond like carbon film of big area.
The present invention solves the technical scheme that above-mentioned first technical problem adopts: this linear ion beam source apparatus, include: negative electrode, anode, be formed with ionization region between described negative electrode and the described anode, be used for ionogenic gas guiding is entered the gas service duct of described ionization region, and the magnet that is used for producing Distribution of Magnetic Field at described ionization region, it is characterized in that: offer an annulus on the described negative electrode, thereby negative electrode is divided into second negative electrode that is in annulus intermediary first negative electrode and is in the periphery, annulus, and also structure ringwise of described anode, and described anode places and corresponding position, the annulus of negative electrode.
The width of the annulus that offers on the described negative electrode is 2～5mm.
The height of described ionization region is 2～5mm.
Described annulus is run-track shaped annulus by what two semicircles and one group of parallel lines were formed.
Described magnet is a permanent magnet, and the N utmost point of this permanent magnet and first negative electrode offset.
Preferably, linear ion beam source apparatus of the present invention also includes cooling water circulation pipeline.
The present invention solves above-mentioned second technical scheme that technical problem adopted: this utilizes the method for above-mentioned linear ion beam source apparatus depositing diamond-like carbon film, adopt the ion sputtering device that workpiece surface is carried out the diamond-like carbon film deposition, it is characterized in that: may further comprise the steps:
Step 1: workpiece is put into acetone or alcohol, utilized ultrasonic cleaning 5～10 minutes,, dry stand-by then with after the rinsed with deionized water;
Step 2: workpiece is placed the vacuum chamber of ion sputtering device, be evacuated to smaller or equal to 2 * 10
-5Behind the Torr, in the gas service duct of linear ion beam source apparatus, feed 35～45sccm rare gas element, simultaneously, the working current of linear ion beam source apparatus is made as 0.1～0.3A, operating voltage is controlled at 1400 ± 50V, simultaneously the negative bias with workpiece be made as-100V～-200V, the working hour is 10～15 minutes;
Step 3: close rare gas element, in the gas service duct of linear ion beam source apparatus, feed 35～45sccm acetylene gas, identical in the power parameter of linear ion beam source apparatus and the step 2, the negative bias of workpiece is made as-100～-200V, the working hour is 10～60 minutes;
Step 4: after thin film deposition finishes, close the power supply of gas and linear ion beam source apparatus, treat that workpiece is cooled to room temperature in vacuum chamber, take out.
Compared with prior art, the invention has the advantages that:
Linear ion beam source apparatus provided by the invention has high plasma body ionization level and ionization energy; No heated filament, plasma body is stable in long-time; Low temperature depositing (＜150 ℃), multiple base material optional (metal, alloy, pottery, plastics, glass etc.); Reactant gases flexible and changeable (argon gas, oxygen, methane, acetylene, silane etc.) can produce the different ions bundle; The most important thing is in larger size range, to produce continuous uniform ion line, be beneficial to the big area uniform deposition.Therefore not only can effectively to remedy the circular ion source of small scale heated filament big because of workpiece dimension for this device, can't be on than big area the defective of uniform deposition diamond like carbon film, can solve also that the magnetron sputtering technique film/basic bonding force is poor, sedimentation rate is low and the with serious pollution problem of surperficial macrobead of cathodic arc technique, be a kind of ideal industrialization multi-function membrane deposition apparatus.
Adopt over-all properties advantages such as method prepared film provided by the invention has the hardness height, film/basic bonding force is good, smooth surface, frictional coefficient is low, thickness is even.
Description of drawings
Fig. 1 is the front view of embodiment of the invention linear ion beam source apparatus;
Fig. 2 be among Fig. 1 A-A to sectional view;
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Linear ion beam source apparatus as shown in Figure 1, comprise negative electrode 1 and anode 2, negative electrode is for being the smooth plate lumphy structure, and offer one on the negative electrode 1 and be run-track shaped annulus 13, thereby negative electrode 1 is divided into second negative electrode 12 that is in annulus intermediary first negative electrode 11 and is in the periphery, annulus, the width of annulus 13 is 5mm, the structure of anode 2 and annulus structural similitude are ringwise, the width of anode 2 is more bigger than the width of annulus, be 5.5mm, and anode 2 places the 13 corresponding positions, annulus with negative electrode 1, and the distance between anode 2 and the negative electrode 1 is 5mm, thereby make to be formed with ionization region 7 between negative electrode 1 and the anode 2, at this moment the height of ionization region 7 is 5mm; Be used for offseting, thereby produce the annular magnetic line of force 6 at the N utmost point and first negative electrode 11 that ionization region 7 produces the magnet permanent magnet 5 of Distribution of Magnetic Field; Also be provided with in addition and be used for ionogenic gas guiding being entered the gas service duct 4 of ionization region 7 and being used for entire equipment is carried out the cooling water circulation pipeline 5 of cooling protection.
During work, working gas is incorporated into ionization region 7 by gas service duct 4, and bumps, decomposes and be ionized at ionization region 7, produces needed plasma body.Utilize the negative bias and the electric field that are added in the ion sputtering device on the workpiece then, thereby ion is drawn from plasma body, form the ion beam current 4 of even continuous large-area, thereby the bombardment workpiece is realized etching pre-washing or deposit film.
In this process, utilize 5 pairs of entire equipment of cooling water circulation pipeline to carry out cooling protection.The linear ion beam source apparatus can feed carbonaceous gas such as methane, acetylene or argon gas, nitrogen, oxygen as working gas, can carry out argon ion etching pre-washing to work piece surface when adopting argon gas; Can realize that nitrogen mixes to work piece surface when adopting nitrogen, adopt oxygen to carry out the oxygen etching work piece surface; Can prepare diamond-like carbon film in work piece surface during carbonaceous gass such as employing methane, acetylene, wherein the magnetic field of permanent magnet generation can increase discharge process electronics and gas molecule collision probability, improves the degree of ionization of working gas.
Utilize above-mentioned linear ion beam source apparatus, adopt the method for ion sputtering device depositing large-area diamond-like carbon film on silicon chip may further comprise the steps:
Step 1: P type (100) monocrystalline silicon piece is put into acetone, utilize ultrasonic cleaning 10min, drying; Clean 10min then in spirituous solution, drying is used deionized water rinsing at last, and dry for standby;
Step 2: silicon chip is fixed on the work supporting block of ion sputtering device, and arranges into the rectangular distribution of 300mm * 100mm, in deposition process, make silicon chip in the work supporting block rotation simultaneously; With mechanical pump and molecular pump the vacuum chamber of ion sputtering device is evacuated to 2 * 10
-5Torr, to the argon gas of linear ion beam source apparatus feeding 40sccm, the working current of linear ion beam source apparatus is made as 0.2A then, and stable operating voltage is at 1400 ± 50V; Negative bias with silicon chip is made as-100V simultaneously; When operating air pressure was 1.2mTorr, depositing time was 10min;
Step 3: close rare gas element, in the gas service duct of linear ion beam source apparatus, feed the 40sccm acetylene gas, identical in the power parameter of linear ion beam source apparatus and the step 2, the negative bias of workpiece is made as-200V, operating air pressure is about 1.4mTorr, and the depositing temperature＜150 ℃ working hour is 60 minutes;
Step 4: after thin film deposition finishes, close the power supply of gas and linear ion beam source apparatus, treat that workpiece is cooled to room temperature in vacuum chamber, take out.
Utilize surface profile step instrument testing film thickness, the institute sedimentary diamond-like carbon film thickness results as shown in Figure 3, the about 10～12nm of longitudinal thickness square root of the variance, uniformity coefficient (square root of the variance/mean value * 100%) is 1.7～2%; About 2～the 4nm of lateral thin-film thickness square root of the variance, uniformity coefficient is 0.4～0.7%.
As follows to sedimentary Properties of Diamond like Carbon test on silicon chip:
Diamond like carbon film nano hardness: 30GPa;
Film/basic bonding force scratching instrument test: 50N;
The frictional coefficient of ball dish frictiograph test class diamond film: 0.1, wearing depth: 0.1 μ m; Test environment is---pair is joined in friction: bearing ball; Linear velocity: 200m/s; Load: 5N; Frictional distance: 500m; Humidity 40～50%, temperature: 20 ± 5 ℃.
Claims (7)
1, a kind of linear ion beam source apparatus, include: negative electrode (1), anode (2), be formed with ionization region (7) between described negative electrode (1) and the described anode (2), be used for ionogenic gas guiding is entered the gas service duct (4) of described ionization region (7), and the magnet (3) that is used for producing Distribution of Magnetic Field at described ionization region (7), it is characterized in that: offer an annulus (13) on the described negative electrode (1), thereby negative electrode (1) is divided into second negative electrode (12) that is in annulus (13) intermediary first negative electrode (11) and is in periphery, annulus (13), and also structure ringwise of described anode (2), and described anode (2) places the corresponding position, annulus (13) with negative electrode (1).
2, linear ion beam source apparatus according to claim 1 is characterized in that: the width of the annulus (13) that offers on the described negative electrode (1) is 2～5mm.
3, linear ion beam source apparatus according to claim 1 and 2 is characterized in that: the height of described ionization region (7) is 2～5mm.
4, linear ion beam source apparatus according to claim 1 and 2 is characterized in that: described annulus (7) are run-track shaped ringwise.
5, according to claim 1 or 2 described linear ion beam source apparatus, it is characterized in that: described magnet (3) is a permanent magnet, and the N utmost point of this permanent magnet and first negative electrode (11) offset.
6, linear ion beam source apparatus according to claim 1 and 2 is characterized in that: also include cooling water circulation pipeline (5).
7, a kind of method of utilizing the described linear ion beam source apparatus of claim 1 depositing diamond-like carbon film adopts the ion sputtering device that workpiece surface is carried out the diamond-like carbon film deposition, it is characterized in that: may further comprise the steps:
Step 1: workpiece is put into acetone or alcohol, utilized ultrasonic cleaning 5～10 minutes,, dry stand-by then with after the rinsed with deionized water;
Step 2: workpiece is placed the vacuum chamber of ion sputtering device, be evacuated to smaller or equal to 2 * 10
-5Behind the Torr, in the gas service duct of linear ion beam source apparatus, feed 35～45sccm rare gas element, simultaneously, the working current of linear ion beam source apparatus is made as 0.1～0.3A, operating voltage is controlled at 1400 ± 50V, simultaneously the negative bias with workpiece be made as-100V～-200V, the working hour is 10～15 minutes;
Step 3: close rare gas element, in the gas service duct of linear ion beam source apparatus, feed 35～45sccm acetylene gas, identical in the power parameter of linear ion beam source apparatus and the step 2, the negative bias of workpiece is made as-100～-200V, the working hour is 10～60 minutes;
Step 4: after thin film deposition finishes, close the power supply of gas and linear ion beam source apparatus, treat that workpiece is cooled to room temperature in vacuum chamber, take out.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792898A (en) * | 2010-04-09 | 2010-08-04 | 中国科学院宁波材料技术与工程研究所 | Carbon film for improving abrasion resistance of magnesium alloy and preparation method thereof |
| CN104294230A (en) * | 2014-10-09 | 2015-01-21 | 中国科学院宁波材料技术与工程研究所 | High-hardness and low-stress multi-element composite diamond-like coating and preparation method thereof |
| CN107686982A (en) * | 2017-08-16 | 2018-02-13 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of super-hydrophobic DLC film |
| CN108315701A (en) * | 2017-01-16 | 2018-07-24 | 中国南玻集团股份有限公司 | The method that coating material and ion beam source deposition prepare coating material |
| CN108374154A (en) * | 2018-02-26 | 2018-08-07 | 温州职业技术学院 | Diamond-like coating preparation facilities with resultant field and its application |
| CN108456883A (en) * | 2017-02-20 | 2018-08-28 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of the carbon-based anti-friction wear-resistant film of matrix surface |
| CN109765257A (en) * | 2012-08-22 | 2019-05-17 | 哈佛学院院长及董事 | Nanoscale scanning sensor |
| CN112126894A (en) * | 2020-09-25 | 2020-12-25 | 中国科学院宁波材料技术与工程研究所 | Ultraviolet-proof plastic film and preparation method and application thereof |
| CN112176406A (en) * | 2020-09-16 | 2021-01-05 | 北京清碳科技有限公司 | Single crystal diamond growth equipment |
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2009
- 2009-05-14 CN CNA2009100987101A patent/CN101550541A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792898A (en) * | 2010-04-09 | 2010-08-04 | 中国科学院宁波材料技术与工程研究所 | Carbon film for improving abrasion resistance of magnesium alloy and preparation method thereof |
| CN109765257A (en) * | 2012-08-22 | 2019-05-17 | 哈佛学院院长及董事 | Nanoscale scanning sensor |
| CN104294230A (en) * | 2014-10-09 | 2015-01-21 | 中国科学院宁波材料技术与工程研究所 | High-hardness and low-stress multi-element composite diamond-like coating and preparation method thereof |
| CN108315701A (en) * | 2017-01-16 | 2018-07-24 | 中国南玻集团股份有限公司 | The method that coating material and ion beam source deposition prepare coating material |
| CN108456883A (en) * | 2017-02-20 | 2018-08-28 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of the carbon-based anti-friction wear-resistant film of matrix surface |
| CN107686982A (en) * | 2017-08-16 | 2018-02-13 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of super-hydrophobic DLC film |
| CN108374154A (en) * | 2018-02-26 | 2018-08-07 | 温州职业技术学院 | Diamond-like coating preparation facilities with resultant field and its application |
| CN112176406A (en) * | 2020-09-16 | 2021-01-05 | 北京清碳科技有限公司 | Single crystal diamond growth equipment |
| CN112126894A (en) * | 2020-09-25 | 2020-12-25 | 中国科学院宁波材料技术与工程研究所 | Ultraviolet-proof plastic film and preparation method and application thereof |
| CN112126894B (en) * | 2020-09-25 | 2023-02-24 | 中国科学院宁波材料技术与工程研究所 | Preparation method of ultraviolet-proof plastic film |
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Open date: 20091007 |