CN103741106A - Ultrathin carbon film prepared with ECR (Electron Cyclotron Resonance) oxygen-argon plasma etching technology and method of preparing ultrathin carbon film - Google Patents
Ultrathin carbon film prepared with ECR (Electron Cyclotron Resonance) oxygen-argon plasma etching technology and method of preparing ultrathin carbon film Download PDFInfo
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 184
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 178
- 238000000034 method Methods 0.000 title claims abstract description 48
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000005516 engineering process Methods 0.000 title claims abstract description 18
- 238000001020 plasma etching Methods 0.000 title abstract 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 164
- 229910052786 argon Inorganic materials 0.000 claims abstract description 93
- 238000005530 etching Methods 0.000 claims abstract description 47
- 238000000151 deposition Methods 0.000 claims abstract description 24
- 239000007789 gas Substances 0.000 claims description 50
- 238000004062 sedimentation Methods 0.000 claims description 44
- -1 argon ion Chemical class 0.000 claims description 32
- 239000011159 matrix material Substances 0.000 claims description 32
- 230000000694 effects Effects 0.000 claims description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 20
- 230000008878 coupling Effects 0.000 claims description 20
- 238000010168 coupling process Methods 0.000 claims description 20
- 238000005859 coupling reaction Methods 0.000 claims description 20
- 239000001301 oxygen Substances 0.000 claims description 20
- 229910052760 oxygen Inorganic materials 0.000 claims description 20
- 238000002294 plasma sputter deposition Methods 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 20
- 230000033001 locomotion Effects 0.000 claims description 11
- 230000000977 initiatory effect Effects 0.000 claims description 10
- 150000001721 carbon Chemical group 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 2
- 230000008021 deposition Effects 0.000 abstract description 10
- 238000004544 sputter deposition Methods 0.000 abstract description 9
- 230000007547 defect Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 105
- 238000004506 ultrasonic cleaning Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 6
- 239000011241 protective layer Substances 0.000 description 4
- 238000005137 deposition process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000005347 demagnetization Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
The invention discloses an ultrathin carbon film prepared with an ECR (Electron Cyclotron Resonance) oxygen-argon plasma etching technology and a method of preparing the ultrathin carbon film. The method is implemented by carrying out sputtering deposition on a carbon film through argon plasma and etching the deposited carbon film with oxygen-argon plasma through an ECR plastic processing system, and has high application value. The defect that a uniform and continuous film cannot be easily formed by directly depositing the ultrathin carbon film is overcome. The ultrathin carbon film prepared with the method is 1.5-3.5 nanometers in thickness, and the surface root mean square roughness is 0.10-0.12 nanometer.
Description
Technical field
The invention belongs to carbon film preparation field, relate to a kind of method of preparing carbon film, be specifically related to ultrathin carbon films and method prepared by a kind of ECR oxygen-argon plasma etch technology.
Background technology
In recent years, carbon film is obtaining application widely with the excellent performance such as its high rigidity, low surface roughness, low-friction coefficient, high-wearing feature, biocompatibility at machinery, electronics, optics, magneticmedium protection and medical field.Wherein, ultrathin carbon films has been brought into play vital effect in magneticmedium protection field.
At present, along with the continuous increase of hard disk magnetic recording density, the yoke distance of hard disk and flying height require constantly to reduce.The magnetic disk surface carbon film protective layer that constantly lowers the requirement of yoke distance is more and more thinner, is about 2～3nm.In addition, under nano level flying height, when hard disk runs into unexpected power-off in operational process or affected by external vibration etc., all may cause between magnetic head and the disk of high speed rotating, mechanical swiping to occur and cause magnetic recording media that demagnetization and loss of data occur.Therefore, the carbon film protective layer of magnetic disk surface must have the surface of ultra-smooth and superior anti-delineation performance.To sum up, the carbon film of preparing ultra-thin, ultra-smooth and having a superior anti-delineation characteristic has important using value and meaning.
Yet the Direct precipitation of ultrathin carbon films still faces very large challenge.In deposition process, first require the carbon can nucleation in any position of matrix surface; Secondly, in deposition process, require carbon surperficial movement not occur for falling low surface energy, make subregion form island structure, and another part region does not have carbon film to cover.This just requires energy particle in deposition process to have suitable energy and higher ionization level.Traditional magnetron sputtering deposition method, because it has lower energy and particle ionization level, is difficult to obtain thickness lower than 2nm and surface uniform continuous thin film.Investigators have proposed to have the filtered cathodic vacuum arc method of high particle ionization level afterwards.Yet, in the plasma body that the method produces, still exist size to be about 1
μthe microparticle carbon of m, this just may introduce defect in the carbon film of deposition, has reduced surfaceness and the performance of carbon film.
Summary of the invention
The object of the invention is to address the above problem the ultrathin carbon films and the method that provide a kind of ECR oxygen-argon plasma etch technology to prepare.The method is utilized electron cyclotron resonace (Electron Cyclotron Resonance, ECR) plasma processing system, by oxygen-argon plasma etch technology, the carbon film having deposited is carried out to attenuate and obtain ultra-thin carbon film, the carbon film of preparation has lower surfaceness and superior anti-delineation performance.
In order to achieve the above object, technical scheme that the present invention adopts is:
ECR oxygen-argon plasma etch technology is prepared a method for ultrathin carbon films, comprises the following steps:
1) utilize ecr plasma system of processing by argon plasma sputtering method, the carbon film that deposit thickness is 3～10nm on matrix;
2) utilize ecr plasma system of processing by oxygen-argon plasma etch method, the carbon film of argon plasma sputtering sedimentation is carried out to etching attenuate, obtain the ultrathin carbon films that thickness is 1.5～3.5nm.
In described step 1), adopt the detailed process of argon plasma sputtering method depositing carbon film on matrix to be:
Matrix is put into plasma chamber, and in cavity, vacuum tightness is extracted into 2 * 10
-4～4 * 10
-4after Pa, pass into argon gas, make the air pressure in chamber be elevated to 2 * 10
-2～6 * 10
-2pa; By applying the magnetic coil electric current of 350～450A and the microwave of 100～300W, make initiating electron in cavity under the coupling of magnetic field and microwave, produce electron cyclotron motion, make the argon gas ionization that passes into, obtain high ionization level, highdensity argon plasma; Apply the direct current (DC) bias of-300～-200V to subsequently carbon target, argon ion in plasma body accelerates bombardment carbon target under the effect of DC negative bias voltage, by transmission ofenergy, to the carbon atom in carbon target, the carbon atom that obtains energy departs from former lattice constraint, to plasma space, discharges; By the substrate bias of apply-30～0V, the argon ion in plasma body drives carbon atom to move and be deposited on matrix surface to matrix and forms carbon film.
Described step 2), in, the employing oxygen-argon plasma etch method etching detailed process of depositing carbon film is:
Stop passing into argon gas, in cavity, pass into oxygen purity and be 5%～20% oxygen and the mixed gas of argon gas, make the air pressure in vacuum chamber be elevated to 2 * 10
-2～6 * 10
-2pa; Under the coupling of the magnetic coil electric current of 350～450A and the microwave of 100～300W, form oxygen-argon plasma equally; It is zero that carbon target direct current (DC) bias is now set, and the oxonium ion in plasma body and argon ion, under the effect of the substrate direct current (DC) bias of-15～-5V, carry out etching attenuate to the carbon film of argon plasma sputtering sedimentation.
In etching process, the etching energy of oxygen-argon plasma is 5～15eV.
The sedimentation rate of argon plasma sputtering sedimentation carbon film and oxygen-argon plasma etch etch rate of depositing carbon film utilize atomic force microscope measurement to calculate; Wherein, sedimentation rate is 3～5nm/min, and etch rate is 0.4～1.0nm/min.
The described detailed process of utilizing atomic force microscope measurement to calculate sedimentation rate and etch rate is:
Before sedimentation, a part for matrix surface is carried out to mask, after sedimentation this part and matrix surface not another part of mask form step, recycling atomic force microscope is measured the height of the step forming, obtain depositing thickness, thereby calculate sedimentation rate according to depositing time;
Before corrasion, a part for film surface is carried out to mask, after corrasion this part and film surface not another part of mask form step, recycling atomic force microscope is measured the degree of depth of the step forming, obtain etching thickness, thereby calculate etch rate according to etching time.
A ultrathin carbon films prepared by ECR oxygen-argon plasma etch technology, the thickness of carbon film is 1.5～3.5nm, surperficial r.m.s. roughness is 0.10～0.12nm.
Compared with prior art, the present invention has following beneficial effect:
The ECR of utilization oxygen-argon plasma etch technology provided by the invention is prepared the method for ultrathin carbon films, utilize ecr plasma system of processing to realize by argon plasma sputtering sedimentation carbon film and oxygen-argon plasma etch two processes of depositing carbon film, overcome the shortcoming that cannot form even continuous film that Direct precipitation ultrathin carbon films easily occurs, there is important using value.
The ultrathin carbon films that the present invention utilizes ECR oxygen-argon plasma etch technology to prepare, its thickness scope is 1.5～3.5nm; The surperficial r.m.s. roughness of ultrathin carbon films is 0.10～0.12nm, in magneticmedium protection field, can meet the requirement of hard disk surface carbon film protective layer effects on surface roughness; The hard disk of uncoated carbon film of take is matrix, and the thickness that the anti-delineation performance of 2.5nm ultrathin carbon films prepared by the present invention is better than Seagate company 7200.12 generation 500G hard disk surface is about the carbon film of 2～4nm.Therefore, the present invention can realize the preparation of ultra-thin ultra-smooth carbon film, especially can be applicable to magneticmedium protection field, realizes the ultra-thin ultra-smooth carbon film in the preparation of high record density hard disk surface with superior anti-delineation performance.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the embodiment of the present invention 1 argon plasma sputtering sedimentation carbon film process;
Fig. 2 is the embodiment of the present invention 1 oxygen-argon plasma etch schematic diagram of depositing carbon film process;
Fig. 3 is the three-dimensional appearance figure of the 2.5nm ultrathin carbon films of the embodiment of the present invention 1 preparation;
The three-dimensional appearance figure of Tu4Wei Seagate company 7200.12 generation 500G hard disk surface carbon film;
Fig. 5 is that 2.5nm carbon film and the Seagate company 7200.12 generation 500G hard disk surface carbon film of the embodiment of the present invention 1 preparation is the cut Cross Section Morphology under 300 μ N at normal load.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is described further:
Embodiment 1
1) referring to Fig. 1, the hard disk of uncoated carbon film of take is matrix, puts into plasma chamber after ultrasonic cleaning, and in cavity, vacuum tightness is extracted into 3 * 10
-4after Pa, pass into argon gas, make the air pressure in vacuum chamber be elevated to 4 * 10
-2pa.Apply the magnetic coil electric current of 420A, open microwave source, regulate microwave power to 200W, the initiating electron in cavity produces electron cyclotron motion and makes the argon gas ionization passing under the coupling of magnetic field and microwave, obtains high ionization level, highdensity argon plasma.After plasmoid is stable, give the direct current (DC) bias of apply-300V of carbon target, the argon ion in plasma body accelerates bombardment carbon target, and under the substrate bias effect of-5V, the carbon laydown in carbon target forms carbon film at matrix surface.The sputtering sedimentation time is 2min, according to sedimentation rate, is 3.5nm/min, and the carbon film thickness that calculates deposition is 7nm.
2) referring to Fig. 2, stop passing into argon gas, the mixed gas that the oxygen that the volume fraction that passes into oxygen in cavity is 12% and argon gas form, makes the air pressure in vacuum chamber be elevated to 4 * 10
-2pa.Under the coupling of the magnetic coil electric current of 420A and the microwave power of 200W, form oxygen-argon hybrid plasma equally.It is zero that carbon target direct current (DC) bias is now set, and the oxonium ion in plasma body (is mainly O
+and O
2 +) and argon ion under the effect of the substrate direct current (DC) bias of-10V, the carbon film of argon plasma sputtering sedimentation is carried out to etching attenuate.Etching time is 10min, according to etch rate, is 0.45nm/min, obtains the ultrathin carbon films that thickness is 2.5nm.In etching process, the etching energy of oxygen-argon plasma is lower, is 10eV, can reduce the damage that corrasion causes disk magnetosphere as far as possible.
3) utilize atomic force microscope to characterize the roughness of the 2.5nm ultrathin carbon films of preparing in the present embodiment and Seagate company 7200.12 generation 500G hard disk surface carbon film, sweep limit is 1 μ m * 1 μ m.Be illustrated in figure 3 the three-dimensional surface shape figure of the carbon film obtaining in the present embodiment, its rough peak diameter is larger, highly less, and r.m.s. roughness is 0.11nm.The three-dimensional appearance figure that is illustrated in figure 4 Seagate company 7200.12 generation 500G hard disk surface carbon film, its rough peak diameter is less, highly higher, and r.m.s. roughness is 0.13nm.Through contrast, can find out; the surfaceness of the carbon film obtaining in the present embodiment is suitable with the roughness of Seagate company 7200.12 generation 500G hard disk surface carbon film, and oxygen-argon plasma etch technology can meet the requirement of hard disk surface carbon film protective layer effects on surface roughness.
Utilize nanometer cut device to characterize the anti-delineation performance of 2.5nm magnetic disk surface ultrathin carbon films in the present embodiment and Seagate company 7200.12 generation 500G hard disk surface carbon film.Concrete, adopt the Berkovich diamond point that radius-of-curvature is 100nm to delineate sample surfaces by applying 300 μ N normal loads.Sample delineation speed is 6 μ m/s, and delineation distance is 150 μ m.After delineation, utilize atomic force microscope to measure the Cross Section Morphology at cut place, obtain scratch depth, thereby contrast the anti-delineation performance of different carbon films.Under identical normal load, scratch depth is less, and its anti-delineation performance is better.Referring to Fig. 5, characterization result shows, the scratch depth of the ultrathin carbon films obtaining in the present embodiment is 1.3nm, and now scratch depth is less than carbon film thickness, and delineation damage occurs in carbon film inside, so just disk magnetosphere is played a very good protection.And contrast Seagate company 7200.12 generation 500G hard disk surface carbon film, its thickness is about 2～4nm, and scratch depth is 2.8nm.Therefore, the Seagate company 7200.12 generation 500G hard disk surface carbon film that compares, the ultrathin carbon films of preparing in the present embodiment has more superior anti-delineation performance.
Embodiment 2
1) take silicon as matrix, put into plasma chamber after ultrasonic cleaning, in cavity, vacuum tightness is extracted into 2 * 10
-4after Pa, pass into argon gas, make the air pressure in vacuum chamber be elevated to 3 * 10
-2pa.Apply the magnetic coil electric current of 350A, open microwave source, regulate microwave power to 100W, the initiating electron in cavity produces electron cyclotron motion and makes the argon gas ionization passing under the coupling of magnetic field and microwave, obtains high ionization level, highdensity argon plasma.After plasmoid is stable, give the direct current (DC) bias of apply-200V of carbon target, the argon ion in plasma body accelerates bombardment carbon target, and under the substrate bias effect of-30V, the carbon laydown in carbon target forms carbon film at matrix surface.The sputtering sedimentation time is 1min, according to sedimentation rate, is 3nm/min, and the carbon film thickness that calculates deposition is 3nm.
2) stop passing into argon gas, the mixed gas that the oxygen that the volume fraction that passes into oxygen in cavity is 20% and argon gas form, makes the air pressure in vacuum chamber be elevated to 5.5 * 10
-2pa.Under the coupling of the magnetic coil electric current of 350A and the microwave power of 300W, form oxygen-argon hybrid plasma.It is zero that carbon target direct current (DC) bias is now set, and the oxonium ion in plasma body (is mainly O
+and O
2 +) and argon ion under the effect of the substrate direct current (DC) bias of-7V, the carbon film of argon plasma sputtering sedimentation is carried out to etching attenuate.Etching time is 1.5min, according to etch rate, is 1nm/min, obtains the ultrathin carbon films that thickness is 1.5nm.In etching process, the etching energy of oxygen-argon plasma is 7eV.
Embodiment 3
1) take the hard disk of uncoated carbon film is matrix, puts into plasma chamber after ultrasonic cleaning, and in cavity, vacuum tightness is extracted into 4 * 10
-4after Pa, pass into argon gas, make the air pressure in vacuum chamber be elevated to 5.5 * 10
-2pa.Apply the magnetic coil electric current of 380A, open microwave source, regulate microwave power to 300W, the initiating electron in cavity produces electron cyclotron motion and makes the argon gas ionization passing under the coupling of magnetic field and microwave, obtains high ionization level, highdensity argon plasma.After plasmoid is stable, give the direct current (DC) bias of apply-280V of carbon target, the argon ion in plasma body accelerates bombardment carbon target, and under the substrate bias effect of-10V, the carbon laydown in carbon target forms carbon film at matrix surface.The sputtering sedimentation time is 2min, according to sedimentation rate, is 5nm/min, and the carbon film thickness that calculates deposition is 10nm.
2) stop passing into argon gas, the mixed gas that the oxygen that the volume fraction that passes into oxygen in cavity is 18% and argon gas form, makes the air pressure in vacuum chamber be elevated to 6 * 10
-2pa.Under the coupling of the magnetic coil electric current of 380A and the microwave power of 180W, form oxygen-argon hybrid plasma.It is zero that carbon target direct current (DC) bias is now set, and the oxonium ion in plasma body (is mainly O
+and O
2 +) and argon ion under the effect of the substrate direct current (DC) bias of-15V, the carbon film of argon plasma sputtering sedimentation is carried out to etching attenuate.Etching time is 13min, according to etch rate, is 0.5nm/min, obtains the ultrathin carbon films that thickness is 3.5nm.In etching process, the etching energy of oxygen-argon plasma is 15eV.
Embodiment 4
1) take the hard disk of uncoated carbon film is matrix, puts into plasma chamber after ultrasonic cleaning, and in cavity, vacuum tightness is extracted into 2.5 * 10
-4after Pa, pass into argon gas, make the air pressure in vacuum chamber be elevated to 2 * 10
-2pa.Apply the magnetic coil electric current of 400A, open microwave source, regulate microwave power to 150W, the initiating electron in cavity produces electron cyclotron motion and makes the argon gas ionization passing under the coupling of magnetic field and microwave, obtains high ionization level, highdensity argon plasma.After plasmoid is stable, give the direct current (DC) bias of apply-220V of carbon target, the argon ion in plasma body accelerates bombardment carbon target, and under the substrate bias effect of-20V, the carbon laydown in carbon target forms carbon film at matrix surface.The sputtering sedimentation time is 2min, according to sedimentation rate, is 3.2nm/min, and the carbon film thickness that calculates deposition is 6.4nm.
2) stop passing into argon gas, the mixed gas that the oxygen that the volume fraction that passes into oxygen in cavity is 10% and argon gas form, makes the air pressure in vacuum chamber be elevated to 2 * 10
-2pa.Under the coupling of the magnetic coil electric current of 420A and the microwave power of 230W, form oxygen-argon hybrid plasma.It is zero that carbon target direct current (DC) bias is now set, and the oxonium ion in plasma body (is mainly O
+and O
2 +) and argon ion under the effect of the substrate direct current (DC) bias of-12V, the carbon film of argon plasma sputtering sedimentation is carried out to etching attenuate.Etching time is 7min, according to etch rate, is 0.6nm/min, obtains the ultrathin carbon films that thickness is 2.2nm.In etching process, the etching energy of oxygen-argon plasma is 12eV.
Embodiment 5
1) take the hard disk of uncoated carbon film is matrix, puts into plasma chamber after ultrasonic cleaning, and in cavity, vacuum tightness is extracted into 3.5 * 10
-4after Pa, pass into argon gas, make the air pressure in vacuum chamber be elevated to 6 * 10
-2pa.Apply the magnetic coil electric current of 420A, open microwave source, regulate microwave power to 270W, the initiating electron in cavity produces electron cyclotron motion and makes the argon gas ionization passing under the coupling of magnetic field and microwave, obtains high ionization level, highdensity argon plasma.After plasmoid is stable, give the direct current (DC) bias of apply-290V of carbon target, the argon ion in plasma body accelerates bombardment carbon target, and under the substrate bias effect of-5V, the carbon laydown in carbon target forms carbon film at matrix surface.The sputtering sedimentation time is 2min, according to sedimentation rate, is 4.5nm/min, and the carbon film thickness that calculates deposition is 9nm.
2) stop passing into argon gas, the mixed gas that the oxygen that the volume fraction that passes into oxygen in cavity is 12% and argon gas form, makes the air pressure in vacuum chamber be elevated to 3.5 * 10
-2pa.Under the coupling of the magnetic coil electric current of 400A and the microwave power of 250W, form oxygen-argon hybrid plasma.It is zero that carbon target direct current (DC) bias is now set, and the oxonium ion in plasma body (is mainly O
+and O
2 +) and argon ion under the effect of the substrate direct current (DC) bias of-10V, the carbon film of argon plasma sputtering sedimentation is carried out to etching attenuate.Etching time is 8min, according to etch rate, is 0.8nm/min, obtains the ultrathin carbon films that thickness is 2.6nm.In etching process, the etching energy of oxygen-argon plasma is 10eV.
Embodiment 6
1) take the hard disk of uncoated carbon film is matrix, puts into plasma chamber after ultrasonic cleaning, and in cavity, vacuum tightness is extracted into 2.8 * 10
-4after Pa, pass into argon gas, make the air pressure in vacuum chamber be elevated to 5 * 10
-2pa.Apply the magnetic coil electric current of 440A, open microwave source, regulate microwave power to 250W, the initiating electron in cavity produces electron cyclotron motion and makes the argon gas ionization passing under the coupling of magnetic field and microwave, obtains high ionization level, highdensity argon plasma.After plasmoid is stable, give the direct current (DC) bias of apply-260V of carbon target, the argon ion in plasma body accelerates bombardment carbon target, and under the substrate bias effect of-10V, the carbon laydown in carbon target forms carbon film at matrix surface.The sputtering sedimentation time is 1min, according to sedimentation rate, is 4nm/min, and the carbon film thickness that calculates deposition is 4nm.
2) stop passing into argon gas, the mixed gas that the oxygen that the volume fraction that passes into oxygen in cavity is 5% and argon gas form, makes the air pressure in vacuum chamber be elevated to 5 * 10
-2pa.Under the coupling of the magnetic coil electric current of 370A and the microwave power of 130W, form oxygen-argon hybrid plasma.It is zero that carbon target direct current (DC) bias is now set, and the oxonium ion in plasma body (is mainly O
+and O
2 +) and argon ion under the effect of the substrate direct current (DC) bias of-8V, the carbon film of argon plasma sputtering sedimentation is carried out to etching attenuate.Etching time is 5min, according to etch rate, is 0.42nm/min, obtains the ultrathin carbon films that thickness is 1.9nm.In etching process, the etching energy of oxygen-argon plasma is 8eV.
Embodiment 7
1) take the hard disk of uncoated carbon film is matrix, puts into plasma chamber after ultrasonic cleaning, and in cavity, vacuum tightness is extracted into 3.3 * 10
-4after Pa, pass into argon gas, make the air pressure in vacuum chamber be elevated to 3.5 * 10
-2pa.Apply the magnetic coil electric current of 450A, open microwave source, regulate microwave power to 220W, the initiating electron in cavity produces electron cyclotron motion and makes the argon gas ionization passing under the coupling of magnetic field and microwave, obtains high ionization level, highdensity argon plasma.After plasmoid is stable, give the direct current (DC) bias of apply-300V of carbon target, the argon ion in plasma body accelerates bombardment carbon target, and under the substrate bias effect of-15V, the carbon laydown in carbon target forms carbon film at matrix surface.The sputtering sedimentation time is 2min, according to sedimentation rate, is 3.6nm/min, and the carbon film thickness that calculates deposition is 7.2nm.
2) stop passing into argon gas, the mixed gas that the oxygen that the volume fraction that passes into oxygen in cavity is 8% and argon gas form, makes the air pressure in vacuum chamber be elevated to 2.5 * 10
-2pa.Under the coupling of the magnetic coil electric current of 450A and the microwave power of 100W, form oxygen-argon hybrid plasma.It is zero that carbon target direct current (DC) bias is now set, and the oxonium ion in plasma body (is mainly O
+and O
2 +) and argon ion under the effect of the substrate direct current (DC) bias of-5V, the carbon film of argon plasma sputtering sedimentation is carried out to etching attenuate.Etching time is 11min, according to etch rate, is 0.4nm/min, obtains the ultrathin carbon films that thickness is 2.8nm.In etching process, the etching energy of oxygen-argon plasma is 5eV.
Embodiment 8
1) take the hard disk of uncoated carbon film is matrix, puts into plasma chamber after ultrasonic cleaning, and in cavity, vacuum tightness is extracted into 2.4 * 10
-4after Pa, pass into argon gas, make the air pressure in vacuum chamber be elevated to 4.5 * 10
-2pa.Apply the magnetic coil electric current of 370A, open microwave source, regulate microwave power to 180W, the initiating electron in cavity produces electron cyclotron motion and makes the argon gas ionization passing under the coupling of magnetic field and microwave, obtains high ionization level, highdensity argon plasma.After plasmoid is stable, give the direct current (DC) bias of apply-240V of carbon target, the argon ion in plasma body accelerates bombardment carbon target, and under the substrate bias effect of-25V, the carbon laydown in carbon target forms carbon film at matrix surface.The sputtering sedimentation time is 2min, according to sedimentation rate, is 3.4nm/min, and the carbon film thickness that calculates deposition is 6.8nm.
2) stop passing into argon gas, the mixed gas that the oxygen that the volume fraction that passes into oxygen in cavity is 15% and argon gas form, makes the air pressure in vacuum chamber be elevated to 4.5 * 10
-2pa.Under the coupling of the magnetic coil electric current of 440A and the microwave power of 280W, form oxygen-argon hybrid plasma.It is zero that carbon target direct current (DC) bias is now set, and the oxonium ion in plasma body (is mainly O
+and O
2 +) and argon ion under the effect of the substrate direct current (DC) bias of-14V, the carbon film of argon plasma sputtering sedimentation is carried out to etching attenuate.Etching time is 4min, according to etch rate, is 0.9nm/min, obtains the ultrathin carbon films that thickness is 3.2nm.In etching process, the etching energy of oxygen-argon plasma is 14eV.
Above content is only explanation technological thought of the present invention; can not limit protection scope of the present invention with this; every technological thought proposing according to the present invention, any change of doing on technical scheme basis, within all falling into the protection domain of the claims in the present invention book.
Claims (7)
- Ultrathin carbon films and method prepared by 1.ECR oxygen-argon plasma etch technology, is characterized in that, comprises the following steps:1) utilize ecr plasma system of processing by argon plasma sputtering method, the carbon film that deposit thickness is 3～10nm on matrix;2) utilize ecr plasma system of processing by oxygen-argon plasma etch method, the carbon film of argon plasma sputtering sedimentation is carried out to etching attenuate, obtain the ultrathin carbon films that thickness is 1.5～3.5nm.
- 2. ECR oxygen-argon plasma etch technology according to claim 1 is prepared the method for ultrathin carbon films, it is characterized in that: in described step 1), adopt the detailed process of argon plasma sputtering method depositing carbon film on matrix to be:Matrix is put into plasma chamber, and in cavity, vacuum tightness is extracted into 2 * 10 -4～4 * 10 -4after Pa, pass into argon gas, make the air pressure in chamber be elevated to 2 * 10 -2～6 * 10 -2pa; By applying the magnetic coil electric current of 350～450A and the microwave of 100～300W, make initiating electron in cavity under the coupling of magnetic field and microwave, produce electron cyclotron motion, make the argon gas ionization that passes into, obtain high ionization level, highdensity argon plasma; Apply the direct current (DC) bias of-300～-200V to subsequently carbon target, argon ion in plasma body accelerates bombardment carbon target under the effect of DC negative bias voltage, by transmission ofenergy, to the carbon atom in carbon target, the carbon atom that obtains energy departs from former lattice constraint, to plasma space, discharges; By the substrate bias of apply-30～0V, the argon ion in plasma body drives carbon atom to move and be deposited on matrix surface to matrix and forms carbon film.
- 3. ECR oxygen-argon plasma etch technology according to claim 1 is prepared the method for ultrathin carbon films, it is characterized in that: described step 2), the employing oxygen-argon plasma etch method etching detailed process of depositing carbon film is:Stop passing into argon gas, in cavity, pass into oxygen purity and be 5%～20% oxygen and the mixed gas of argon gas, make the air pressure in vacuum chamber be elevated to 2 * 10 -2～6 * 10 -2pa; Under the coupling of the magnetic coil electric current of 350～450A and the microwave of 100～300W, form oxygen-argon plasma equally; It is zero that carbon target direct current (DC) bias is now set, and the oxonium ion in plasma body and argon ion, under the effect of the substrate direct current (DC) bias of-15～-5V, carry out etching attenuate to the carbon film of argon plasma sputtering sedimentation.
- 4. ECR oxygen-argon plasma etch technology according to claim 3 is prepared the method for ultrathin carbon films, it is characterized in that: in etching process, the etching energy of oxygen-argon plasma is 5～15eV.
- 5. ECR oxygen-argon plasma etch technology according to claim 1 is prepared the method for ultrathin carbon films, it is characterized in that: the sedimentation rate of argon plasma sputtering sedimentation carbon film and oxygen-argon plasma etch etch rate of depositing carbon film utilize atomic force microscope measurement to calculate; Wherein, sedimentation rate is 3～5nm/min, and etch rate is 0.4～1.0nm/min.
- 6. ECR oxygen-argon plasma etch technology according to claim 5 is prepared the method for ultrathin carbon films, it is characterized in that: the described detailed process of utilizing atomic force microscope measurement to calculate sedimentation rate and etch rate is:Before sedimentation, a part for matrix surface is carried out to mask, after sedimentation this part and matrix surface not another part of mask form step, recycling atomic force microscope is measured the height of the step forming, obtain depositing thickness, thereby calculate sedimentation rate according to depositing time;Before corrasion, a part for film surface is carried out to mask, after corrasion this part and film surface not another part of mask form step, recycling atomic force microscope is measured the degree of depth of the step forming, obtain etching thickness, thereby calculate etch rate according to etching time.
- 7. the ultrathin carbon films that prepared by the method described in employing claim 1 to 6 any one claim, is characterized in that: the thickness of ultrathin carbon films is 1.5～3.5nm, surperficial r.m.s. roughness is 0.10～0.12nm.
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