CN112858730A - Diamond-like coated atomic force microscope probe and preparation method thereof - Google Patents
Diamond-like coated atomic force microscope probe and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a diamond-like coated atomic force microscope probe and a preparation method thereof, relating to the technical field of atomic force microscope probes.
Description
Technical Field
The invention relates to the technical field of atomic force microscope probes, in particular to a diamond-like coated atomic force microscope probe and a preparation method thereof.
Background
The operating principle of Atomic Force Microscopy (AFM) is based on the interaction of a sharp tip, typically made of Si or Si, with the atomic-scale loading of the sample surface to obtain topographical information about the surface3N4The probe is processed by MEMS process, the radius of the probe tip is dozens of nanometers, and some special probes are coated with 10-50nm thick metal Pt or ferromagnetic materials such as Co, Fe and the like on the surfaceObtaining the conductive probe or the magnetic probe. However, the probe is continuously worn during the scanning of the sample surface, and the film layer on the probe surface is easily peeled off, resulting in a decrease in measurement accuracy and an error. Therefore, it is important to reduce wear of the AFM tip during the experiment to extend its useful life.
At present, in order to improve the service life of the AFM tip, some researchers have proposed that the AFM tip is coated with a graphene material to improve the service life of the tip. For example, patent CN104360107A discloses the use of an immersion method to coat graphene on the tip of AFM. However, the coating yield of the graphene prepared by the method is not high, and van der waals force is combined between the graphene and the needle point, so that an uncoated area exists on the needle point, and the graphene layer is easy to fall off from the needle point in the using process, so that the failure of a film layer is caused.
In the liquid phase transfer method disclosed in patent CN108375687A, an AFM tip is first immersed in a polylysine aqueous solution for surface modification, and then immersed in a graphene solution, so as to obtain a graphene-coated AFM tip. According to the method, the interaction between polycations in polylysine and anions on graphene increases the acting force between the graphene and the needle point, but the graphene film prepared by the method is in an atomic layer level, is single-layer or thin-layer graphene, the bonding force between the graphene film and a substrate is still weak, and the coverage rate of the prepared graphene on the needle point cannot be controlled.
Disclosure of Invention
The invention provides a diamond-like coated atomic force microscope probe and a preparation method thereof, aiming at solving the problems that the probe is continuously worn in the process of scanning the surface of a sample, a film layer on the surface of the probe is easy to fall off, the measurement precision is reduced, errors are caused and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a diamond-like coated atomic force microscope probe comprises a substrate and a needle tip arranged at the end part of the substrate, wherein the needle tip is coated with a diamond-like film.
The invention coats the diamond-like film on the surface of the probe tip of the atomic force microscope, endows the atomic force microscope probe with excellent mechanical property, thermal stability and chemical stability, and can obviously prolong the service life and performance of the AFM probe.
Preferably, the diamond-like thin film has a thickness of 10 to 100 nm.
A preparation method of an atomic force microscope probe coated by diamond-like carbon is characterized by comprising the following steps:
(1) cleaning: cleaning the atomic force microscope probe to be coated, and then drying the probe for later use;
(2) and (3) activation: fixing the atomic force microscope probe to be coated in a uniform plasma source sputtering chamber, and then activating and cleaning the surface of the needle tip;
(3) depositing and coating a diamond-like film: and performing magnetron sputtering deposition on the needle point by taking carbon as a target material.
The invention takes carbon as a target material, adopts a magnetron sputtering method to deposit and coat the diamond-like film on the probe point of the atomic force microscope, is suitable for the atomic force microscope probes with different sizes and specifications, can realize the preparation of the diamond-like film on the probe point of the atomic force microscope with low cost, high adhesion and high coverage, and has high film-substrate binding force, controllable film deposition rate, batch production and no environmental pollution.
Preferably, in the step (1), the ultrasonic cleaning is sequentially carried out by using acetone, ethanol and plasma water, and then the drying is carried out by using nitrogen.
Preferably, the activation washing in step (2) is at 4.0X 10-4-6.0×10-4And (3) under Pa, activating and cleaning the surface of the needle point for 25-35min by adopting argon plasma.
Before the diamond-like carbon film is deposited, argon is firstly introduced, a direct current power supply is turned on, the surface of the needle point is activated and cleaned through argon plasma, and an oxide layer and pollutants on the surface of the needle point can be removed after the activation and cleaning, so that the binding force between the film and the surface of the needle point is improved.
Preferably, the uniform plasma source sputtering chamber comprises a cavity, a plurality of air inlets are formed in the periphery of the cavity, and a probe rotating table is arranged in the cavity.
Preferably, the aperture of the air inlet is 5-10 mm.
Preferably, the magnetron sputtering deposition conditions in step (3): the deposition bias is-20V to 140V, the vacuum degree is 0.1 to 0.3Pa, the target power is 1 to 3kW, and the deposition time is 3 to 10 min.
Preferably, the heating temperature of the needle tip in the magnetron sputtering deposition in the step (3) is 60-230 ℃.
Preferably, in the step (3), the vertical distance between the tip of the needle tip and the gas inlet is 10-15cm, the rotating speed is 1-20rpm, the sputtering gas is argon gas, and the flow rate of the argon gas is 10-30 sccm.
When the magnetron sputtering is used for depositing and coating the diamond-like film on the needle point, parameters such as deposition bias voltage, vacuum degree, target material power and the like need to be strictly controlled, and because the needle point of the atomic force microscope probe is of a high aspect ratio structure, the situation of uneven deposition is very easy to occur on the tapered section of the needle point in the deposition process, the needle point needs to be heated during deposition so as to improve the mobility of sputtered particles, the temperature needs to be controlled between 60 ℃ and 230 ℃, if the temperature is too low, the effect of improving the mobility of the sputtered particles cannot be effectively achieved, and if the temperature is too high, the crystal grains of the film are large, the thermal stress is increased, the film is easy to crack, and the quality of the film is influenced; and during deposition, the needle point needs to be subjected to rotary deposition through the probe rotary table so as to achieve the purpose of uniform deposition. Meanwhile, in the experimental process, the inventor further discovers that due to the characteristic of high aspect ratio of the needle point, high coverage deposition at the tip end of the needle point cannot be guaranteed only by heating and rotating, in order to enable the tip end of the needle point to be uniformly deposited, the invention adopts the self-designed uniform plasma source sputtering chamber to carry out magnetron sputtering, a plurality of air inlets are arranged at equal intervals around the uniform plasma source sputtering chamber and used for introducing argon to deposit the diamond-like film, and meanwhile, through a large number of experimental researches, the aperture of the air inlets, the vertical distance between the tip end of the needle point and the air inlets during magnetron sputtering deposition, the rotating speed and the argon flow rate are strictly controlled, so that the tip end of the needle point can be uniformly deposited.
Therefore, the invention has the following beneficial effects:
(1) according to the invention, the surface of the probe tip of the atomic force microscope is coated with the diamond-like film, so that the atomic force microscope probe has excellent mechanical property, thermal stability and chemical stability, and the service life and performance of the AFM probe can be obviously prolonged;
(2) the invention adopts the magnetron sputtering method to carry out diamond-like film deposition coating on the probe point of the atomic force microscope probe, is suitable for the atomic force microscope probes with different sizes and specifications, can realize the low-cost, high-adhesion and high-coverage preparation of the diamond-like film on the probe point of the atomic force microscope probe, and has high film-substrate binding force, controllable film deposition rate, batch production and no environmental pollution;
(2) the invention combines the parameter limitation and the specially designed uniform plasma source sputtering chamber with the needle point heating, and the prepared diamond-like carbon film can be uniformly deposited and coated on the needle point with a high aspect ratio structure.
Drawings
FIG. 1 is a schematic diagram of the probe structure of an atomic force microscope of the present invention.
FIG. 2 is a schematic diagram of a sputtering chamber of a uniform plasma source according to the present invention.
FIG. 3 is a schematic cross-sectional view of a sputtering chamber of a uniform plasma source according to the present invention.
FIG. 4 is an atomic force microscope image of the diamond-like carbon film prepared in example 1 of the present invention.
In the figure: the device comprises a substrate 1, a needle tip 2, a diamond-like carbon film 3, a uniform plasma source sputtering chamber 4, a cavity 5, an air inlet 6 and a probe rotating platform 7.
Detailed Description
The invention is further described with reference to specific embodiments.
General example: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 10-100 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 4.0 multiplied by 10-4 -6.0×10-4Activating and cleaning the surface of the needle tip for 25-35min by adopting argon plasma under Pa;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 10-15cm, the rotating speed is 1-20rpm, the sputtering gas is argon, the flow rate of the argon is 10-30sccm, the deposition bias is-20V-140V, the vacuum degree is 0.1-0.3Pa, the power of the target material is 1-3kW, the heating temperature of the needle point is 60-230 ℃, and the deposition time is 3-10 min;
the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating platform 7 is arranged in the cavity, and the aperture of each air inlet is 5-10 mm.
Example 1: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.0 multiplied by 10-4In the following, argon plasma is usedActivating and cleaning the surface of the needle point for 30 min;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-80V, the vacuum degree is 0.2Pa, the target material power is 2kW, the heating temperature of the needle point is 150 ℃, and the deposition time is 7 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Example 2: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 10 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 4.0 multiplied by 10-4Activating and cleaning the surface of the needle tip for 35min by adopting argon plasma under Pa;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 10cm, the rotating speed is 15rpm, the sputtering gas is argon, the argon flow rate is 10sccm, the deposition bias voltage is-140V, the vacuum degree is 0.1Pa, the target material power is 3kW, the heating temperature of the needle point is 60 ℃, and the deposition time is 3 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 10 mm.
Example 3: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 100 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 6.0 multiplied by 10-4Activating and cleaning the surface of the needle point for 33min by adopting argon plasma under Pa;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 15cm, the rotating speed is 20rpm, the sputtering gas is argon, the argon flow rate is 30sccm, the deposition bias voltage is-20V, the vacuum degree is 0.3Pa, the target material power is 1kW, the heating temperature of the needle point is 230 ℃, and the deposition time is 10 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 5 mm.
Example 4: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 80 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.5 multiplied by 10-4Activating and cleaning the surface of the needle tip for 27min by adopting argon plasma under Pa;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 10cm, the rotating speed is 5rpm, the sputtering gas is argon, the argon flow rate is 30sccm, the deposition bias voltage is-100V, the vacuum degree is 0.3Pa, the target material power is 3kW, the heating temperature of the needle point is 200 ℃, and the deposition time is 5 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 7 mm.
Example 5: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 20 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 4.0 multiplied by 10-4Activating and cleaning the surface of the needle tip for 28min by adopting argon plasma under Pa;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 13cm, the rotating speed is 2rpm, the sputtering gas is argon, the argon flow rate is 15sccm, the deposition bias voltage is-40V, the vacuum degree is 0.15Pa, the target material power is 1.8kW, the heating temperature of the needle point is 120 ℃, and the deposition time is 4 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Comparative example 1: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.0 multiplied by 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-80V, the vacuum degree is 0.2Pa, the target material power is 2kW, the heating temperature of the needle point is 150 ℃, and the deposition time is 7 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Comparative example 2: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.0 multiplied by 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-10V, the vacuum degree is 0.2Pa, the target material power is 5kW, the heating temperature of the needle point is 150 ℃, and the deposition time is 7 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Comparative example 3: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.0 multiplied by 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the flow rate of the argon is 40sccm, the deposition bias voltage is-170V, the vacuum degree is 0.4Pa, the target material power is 4kW, the heating temperature of the needle point is 150 ℃, and the deposition time is 7 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Comparative example 4: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.0 multiplied by 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-180V, the vacuum degree is 0.2Pa, the target material power is 0.5kW, the heating temperature of the needle point is 150 ℃, and the deposition time is 7 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Comparative example 5: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.0 multiplied by 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-80V, the vacuum degree is 0.2Pa, the target material power is 5kW, the heating temperature of the needle point is 150 ℃, and the deposition time is 7 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Comparative example 6: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.0 multiplied by 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-170V, the vacuum degree is 0.2Pa, the target material power is 2kW, the heating temperature of the needle point is 150 ℃, and the deposition time is 7 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Comparative example 7: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated was fixed in a common chamber and then heated at 5.0X 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: and performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and the air inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-80V, the vacuum degree is 0.2Pa, the target material power is 2kW, the needle point is not heated, and the deposition time is 7 min.
Comparative example 8: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated was fixed in a common chamber and then heated at 5.0X 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: and performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and the gas inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-80V, the vacuum degree is 0.2Pa, the target material power is 2kW, the heating temperature of the needle point is 150 ℃, and the deposition time is 7 min.
Comparative example 9: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.0 multiplied by 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-80V, the vacuum degree is 0.2Pa, the target material power is 2kW, the needle point is not heated, and the deposition time is 7 min;
the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Comparative example 10: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.0 multiplied by 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-80V, the vacuum degree is 0.2Pa, the target material power is 2kW, the heating temperature of the needle point is 260 ℃, and the deposition time is 7 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Comparative example 11: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.0 multiplied by 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 18cm, the rotating speed is 10rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-80V, the vacuum degree is 0.2Pa, the target material power is 2kW, the heating temperature of the needle point is 150 ℃, and the deposition time is 7 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Comparative example 12: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.0 multiplied by 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 12cm, the rotating speed is 30rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-80V, the vacuum degree is 0.2Pa, the target material power is 2kW, the heating temperature of the needle point is 150 ℃, and the deposition time is 7 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Comparative example 13: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: the atomic force microscope probe to be coated is fixed in a sputtering chamber of a uniform plasma source and then is positioned at 5.0 multiplied by 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the argon flow rate is 20sccm, the deposition bias voltage is-80V, the vacuum degree is 0.2Pa, the target material power is 2kW, the heating temperature of the needle point is 150 ℃, and the deposition time is 7 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 14 mm.
Comparative example 14: a kind of atom force microscope probe coated with diamond, including the basement 1 and locating the tip 2 of basal end, the said tip is coated with the diamond-like film 3, the thickness of the said diamond-like film is 50 nm;
a preparation method of a diamond-like coated atomic force microscope probe comprises the following steps:
(1) cleaning: ultrasonic cleaning the atomic force microscope probe to be coated by sequentially adopting acetone, ethanol and plasma water, and then drying by adopting nitrogen for later use;
(2) and (3) activation: fixing the atomic force microscope probe to be coated on a uniform plasma sourceIn the shooting chamber, then at 5.0X 10-4Then, activating and cleaning the surface of the needle point for 30min by adopting argon plasma;
(3) depositing and coating a diamond-like film: performing magnetron sputtering deposition on the needle point by taking carbon as a target material, wherein the vertical distance between the tip of the needle point and an air inlet during deposition is 12cm, the rotating speed is 10rpm, the sputtering gas is argon, the flow rate of the argon is 5sccm, the deposition bias voltage is-80V, the vacuum degree is 0.2Pa, the target material power is 2kW, the heating temperature of the needle point is 150 ℃, and the deposition time is 7 min; the uniform plasma source sputtering chamber 4 comprises a cavity 5, a plurality of air inlets 6 are formed in the periphery of the cavity, a probe rotating table 7 is arranged in the cavity, and the aperture of each air inlet is 8 mm.
Testing the appearance, hardness, friction performance, thermal stability and chemical stability of the diamond-like carbon film by using the diamond-like carbon coated atomic force microscope probe prepared in the embodiment and the comparative example; wherein, the hardness is tested by adopting a nano-indenter under the following test conditions: setting 1/10 of the film thickness as a loading depth, taking at least 16 test points for each sample, and finally taking an average value; the friction performance test load is 2N, the sliding speed is 5cm/s, and the test time is 40 minutes; the thermal stability is that the film is subjected to thermal annealing treatment at the temperature of 200 ℃; the chemical stability is that the prepared DLC film is placed in an atmospheric environment for 2 years, and then hardness and friction performance tests are carried out. The results are shown below.
FIG. 4 is a diagram of the morphology of the diamond-like carbon film AFM prepared in example 1, which shows that the roughness Rq of the diamond-like carbon film prepared is 0.83nm, and the surface of the film has nanoscale flatness, so that the test application process of the diamond-like carbon coated AFM probe is not affected.
According to the data, the diamond-like carbon coated atomic force microscope probe prepared by the embodiment of the invention has excellent mechanical property, friction property, thermal stability and chemical stability; the comparative examples 1 to 6 are different from example 1 in that the deposition bias, the degree of vacuum and the target power are not simultaneously controlled within the limited ranges, and thus they cannot simultaneously have excellent mechanical properties, frictional properties, thermal stability and chemical stability; comparative example 7 is different from example 1 in that the tip of the probe is not heated and a specially designed chamber is not adopted, comparative example 8 is different from example 1 in that only the tip of the probe is heated and a specially designed chamber is not adopted, and comparative example 9 is different from example 1 in that a specially designed chamber is adopted but the tip of the probe is not heated, so that a uniform diamond-like film cannot be obtained through good deposition, and the mechanical property of the probe is poor, the friction coefficient is high, and the thermal stability and the chemical stability are also poor; the comparative example 10 is different from the example 1 in that the heating temperature of the needle tip is too high, so that the crystal grains of the film are coarse, the thermal stress is increased, and the film is easy to crack; comparative examples 11 to 14 are different from example 1 in that the vertical distance between the tip end of the needle and the gas inlet at the time of deposition, the rotation speed, the flow rate of argon gas, or the aperture of the gas inlet was not controlled within a limited range, and the performance of the deposited film was relatively poor.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. The atomic force microscope probe coated with the diamond-like carbon is characterized by comprising a substrate and a needle point arranged at the end part of the substrate, wherein the needle point is coated with a diamond-like carbon film.
2. The diamond-like coated afm probe of claim 1, wherein the diamond-like thin film has a thickness of 10-100 nm.
3. A method of preparing a diamond-like coated atomic force microscope probe according to claim 1, comprising the steps of:
(1) cleaning: cleaning the atomic force microscope probe to be coated, and then drying the probe for later use;
(2) and (3) activation: fixing the atomic force microscope probe to be coated in a uniform plasma source sputtering chamber, and then activating and cleaning the surface of the needle tip;
(3) depositing and coating a diamond-like film: and performing magnetron sputtering deposition on the needle point by taking carbon as a target material.
4. The method for preparing a diamond-like coated AFM probe according to claim 3, wherein the step (1) comprises ultrasonic cleaning with acetone, ethanol, plasma water, and blow-drying with nitrogen.
5. The method of claim 3, wherein the step (2) of activating and cleaning is performed at 4.0 x 10-4 -6.0×10-4 And (3) under Pa, activating and cleaning the surface of the needle point for 25-35min by adopting argon plasma.
6. The method according to claim 3, wherein the sputtering chamber of the homogeneous plasma source comprises a cavity, the cavity has a plurality of gas inlets around the cavity, and the cavity has a probe rotation stage inside.
7. The method of claim 6, wherein the aperture of the gas inlet is 5-10 mm.
8. The method for preparing a diamond-like coated AFM probe according to claim 3, wherein the magnetron sputtering deposition conditions in step (3): the deposition bias is-20V to 140V, the vacuum degree is 0.1 to 0.3Pa, the target power is 1 to 3kW, and the deposition time is 3 to 10 min.
9. The method for preparing a diamond-like coated AFM probe as claimed in claim 3, wherein the heating temperature of the needle tip in step (3) is 60-230 ℃.
10. The method for preparing a diamond-like coated AFM probe as claimed in claim 3, wherein the perpendicular distance between the tip of the needle and the gas inlet in the magnetron sputtering deposition in step (3) is 10-15cm, the rotation speed is 1-20rpm, the sputtering gas is argon gas, and the flow rate of the argon gas is 10-30 sccm.
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