CN108878260B - Low-friction fluorine-containing onion carbon film and method for directly preparing same on silicon substrate - Google Patents
Low-friction fluorine-containing onion carbon film and method for directly preparing same on silicon substrate Download PDFInfo
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Abstract
The invention provides a low-friction fluorine-containing onion carbon film and a method for directly preparing the same on a silicon substrate. The onion carbon prepared by the method has the advantages of high purity, simple process, simple and convenient operation, low cost, low energy consumption, good controllability, mass production, obvious economic benefit and the like, and the onion carbon contains fluorine capable of reducing the surface energy, so that the tribological performance of the material can be greatly improved, and the onion carbon is suitable for lubricating silicon-based MEMS/NEMS parts.
Description
Technical Field
The invention relates to the technical field of low-friction fluorine-containing onion carbon films and preparation of onion carbon, in particular to a preparation technology of a fluorine-containing onion carbon film, and particularly relates to a preparation method of a low-friction fluorine-containing onion carbon film directly used for silicon-based MEMS/NEMS.
Background
Onion carbon is an allotrope of carbon, consisting of multiple layers of closed quasi-spherical graphite, having a unique spherical nanostructure and high chemical inertness. These advantages make it particularly advantageous for tribological applications. At present, the preparation method of nano onion carbon can be mainly divided into physical methods (such as arc discharge method, plasma method and electron beam radiation method) and chemical methods (such as chemical vapor deposition method, nano diamond vacuum heat treatment method and pyrolysis method). However, these methods have high requirements on raw materials, equipment and process condition control, and have the problems of complicated operation, poor controllability and the like. According to the invention patent with the application number of CN201310314469, the nano onion carbon is prepared by adopting a liquid jet method; the carbon black is used as a raw material, and the nano onion carbon can be obtained through the steps of dispersing, pressurizing and micronizing, drying, grinding and the like. The method has the advantages of complex process, lower yield and poor controllability. Further, as in the patent application with application No. CN201610159997, it is proposed to prepare onion carbon at high temperature and high pressure; the nano-scale carbon onion powder is prepared by using nano-diamond powder as a raw material, briquetting, assembling, treating at high temperature (1273-1773K) and high pressure (1.0-5.2 GPa), cooling, releasing pressure and grinding. The method has high equipment cost, harsh process conditions and high energy consumption, and the product is often accompanied by impurity phases and is difficult to separate. In addition, the onion carbon prepared by the two methods is powdery, and when the onion carbon is applied to the surface of a material for friction reduction and wear resistance, the onion carbon needs to be coated, filled or assembled, and the like, so that time and labor are wasted, the surface roughness of the material is large, and the friction reduction and wear resistance are reduced to some extent. The invention patent application with the application number of CN201711361086 adoptsThe use of plasma chemical vapor deposition to produce onion carbon on stainless steel sheeting, while providing some improvement in tribological properties, is expensive and requires a vacuum of up to 10 f-4Firstly, argon ion bombardment cleaning is carried out (bias voltage is 800-; then depositing for 2-4 hours under the pulse bias of 1200-1500V by using methane or acetylene as a carbon source. High cost, high energy consumption, complex operation and long deposition time.
Disclosure of Invention
The purpose of the invention is realized as follows: firstly, preparing an organic molecular film by adopting an environment-friendly, simple and feasible electrophoretic deposition technology, and then carrying out annealing heat treatment on the molecular film, thereby obtaining the onion carbon with low cost, high purity and good controllability. In order to overcome the defects of complex process, complex operation, high cost, high energy consumption, impurity phase accompanied, low controllability and the like in the existing onion carbon preparation technology; the invention provides a method for directly preparing a low-friction fluorine-containing onion carbon film on a silicon substrate, wherein an organic molecular film is prepared by an anodic electrophoresis method, and the onion carbon is prepared by annealing treatment. Most importantly, the uniform and smooth onion carbon film can be directly prepared on the silicon substrate, which is beneficial to reducing the friction coefficient and the wear rate of the material and is particularly suitable for lubricating micro parts such as MEMS/NEMS.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the method for directly preparing the low-friction fluorine-containing onion carbon film on the silicon substrate is characterized in that the molecular film deposited by the annealing electrophoresis method is directly used for preparing the low-friction fluorine-containing onion carbon on the silicon substrate, and the method comprises the following steps:
(1) using 98% H with volume ratio of 7:32SO4And 30% H2O2Cleaning the silicon wafer by using the mixed solution, then cleaning the silicon wafer for several times by using ultrapure water, and finally drying the silicon wafer by using nitrogen;
(2) placing two silicon wafers in parallel face to face, immersing the two silicon wafers into an organic monocarboxylic acid aqueous solution to be used as a working electrode and a counter electrode respectively, and then connecting two ends of the two silicon wafers with the positive electrode and the negative electrode of a direct current power supply respectively;
(3) electrifying a working electrode and a counter electrode, and depositing a film on the surface of the silicon wafer by adopting an electrophoresis method;
(4) and annealing the prepared film under the protection of inert gas.
Further, the silicon wafer used was an N-type polished single crystal silicon wafer having a crystal orientation of < 100 > and a resistivity of 0.001 to 1.5. omega. m.
Furthermore, the distance between the two silicon wafers as the working electrode and the counter electrode is 2-20 mm.
Further, the organic monocarboxylic acid is one of trifluoroacetic acid, trifluoropropionic acid, heptafluorobutyric acid, pivalic acid, undecafluorohexanoic acid, perfluoroheptanoic acid, and the like.
Further, the concentration of the aqueous solution of the organic monocarboxylic acid is 0.5 to 10 mmol/L.
Further, the voltage is 5-50V during the process of depositing the film by the electrophoresis method.
Further, the deposition time of the electrophoretic method for depositing the film is 10-120 min.
Further, the inert protective gas is one or more of nitrogen, argon and helium.
Furthermore, the annealing temperature of the film is 300-.
The low-friction fluorine-containing onion carbon film prepared by the method for directly preparing the low-friction fluorine-containing onion carbon film on the silicon substrate is characterized in that the prepared carbon film is of an onion structure and contains fluorine.
Organic monocarboxylic acids readily ionize carboxylate anions in aqueous solution. Therefore, carboxylate anions can move to the anode when being in a uniform electric field, so that the organic carboxylic acid molecular film is prepared by using an anodic electrophoretic deposition technology. This is a purely physical process without altering the structure and composition of the molecule. And (3) annealing the deposited organic carboxylic acid molecular film under the protection of gas to completely decompose the organic molecular film, wherein carbonyl groups in the organic carboxylic acid molecular film can escape in the form of carbon dioxide and water, so that carbon atoms are rearranged to form onion carbon.
The invention has the beneficial effects that the preparation method is novel, the onion carbon is prepared by adopting a two-step method of electrophoretic deposition and annealing treatment, and the tribological property of the onion carbon is further improved by doping fluorine in the onion carbon. Because the anode electrophoretic deposition technology is adopted, no metal ions are deposited on the anode, the prepared onion carbon has high purity, good controllability, uniform and smooth film, low raw material cost, simple equipment, simple process, low energy consumption, easy operation, time and labor conservation and excellent tribological performance. The defects of high cost of raw materials and equipment, complex process, high energy consumption, complex operation, time and labor waste, low purity, poor controllability, poor friction-reducing and wear-resisting properties and the like in the conventional onion carbon preparation are overcome, and the method has the advantages of large-batch production, remarkable economic benefit and the like and is suitable for lubricating MEMS/NEMS parts.
Drawings
FIG. 1 is a transmission electron microscope image of a fluorine-containing onion carbon film prepared in example 3;
FIG. 2 is a Raman spectrum of the carbon film containing fluorine onion prepared in example 3;
FIG. 3 is an X-ray photoelectron spectrum of the carbon film containing fluorine onion prepared in example 3.
Detailed Description
The invention will be further described with reference to the following figures and specific examples, but the scope of the invention is not limited thereto.
[ example 1 ]
(1) An N-type polished monocrystalline silicon wafer with the crystal orientation of < 100 > and the resistivity of 0.01 omega-m is cut into two small silicon wafers of 1cm multiplied by 2cm by a diamond cutter.
(2) The silicon wafer of the above size was put in a chamber containing 98% H in a volume ratio of 7:32SO4And 30% H2O2And cleaning the silicon wafer in a wide-mouth bottle of the mixed solution by using an ultrasonic cleaner, then cleaning the silicon wafer for several times by using ultrapure water, and finally drying the silicon wafer by using nitrogen.
(3) Two silicon wafers are clamped by a clamp, are arranged in parallel face to face at a distance of 5mm, are respectively used as a working electrode and a counter electrode, are immersed into a container containing trifluoroacetic acid aqueous solution with the concentration of 3mmol/L, and then the two ends of the clamp are respectively connected with the positive electrode and the negative electrode of a direct current power supply.
(4) A voltage of 20V was used to deposit the film for 30 minutes.
(5) The prepared film is annealed for 60 minutes at 800 ℃ under the protection of nitrogen. And then cooling to room temperature under the protection of gas to obtain the A film.
A friction tester is utilized, a steel ball is used as a friction matching pair, a friction experiment is carried out under the conditions that the load is 0.05N, the linear speed is 0.02m/s, and the testing time is 30min, and the tribological performance of the film is inspected by a three-dimensional surface profiler.
[ example 2 ]
(1) An N-type polished monocrystalline silicon wafer with a crystal orientation of < 100 > and a resistivity of 0.01 omega-m was cut into two small silicon wafers of 1cm × 2cm size with a diamond knife.
(2) The silicon wafer of the above size was put in a chamber containing 98% H in a volume ratio of 7:32SO4And 30% H2O2And cleaning the silicon wafer in a wide-mouth bottle of the mixed solution by using an ultrasonic cleaner, then cleaning the silicon wafer for several times by using ultrapure water, and finally drying the silicon wafer by using nitrogen.
(3) Two silicon wafers are clamped by a clamp, are arranged in parallel face to face at a distance of 5mm, are respectively used as a working electrode and a counter electrode, are immersed into a container containing trifluoroacetic acid aqueous solution with the concentration of 3mmol/L, and then the two ends of the clamp are respectively connected with the positive electrode and the negative electrode of a direct current power supply.
(4) A voltage of 25V was used to deposit the film for 30 minutes.
(5) And annealing the prepared film at 800 ℃ for 60 minutes under the protection of argon. And then cooling to room temperature under the protection of gas to obtain a B film.
A friction tester is utilized, a steel ball is used as a friction matching pair, a friction experiment is carried out under the conditions that the load is 0.05N, the linear speed is 0.02m/s, and the testing time is 30min, and the tribological performance of the film is inspected by a three-dimensional surface profiler.
[ example 3 ]
(1) An N-type polished monocrystalline silicon wafer with a crystal orientation of < 100 > and a resistivity of 0.01 omega-m was cut into two small silicon wafers of 1cm × 2cm size with a diamond knife.
(2) The silicon wafer of the above size was put in a chamber containing 98% H in a volume ratio of 7:32SO4And 30% H2O2And cleaning the silicon wafer in a wide-mouth bottle of the mixed solution by using an ultrasonic cleaner, then cleaning the silicon wafer for several times by using ultrapure water, and finally drying the silicon wafer by using nitrogen.
(3) Two silicon wafers are clamped by a clamp, are arranged in parallel face to face at a distance of 5mm, are respectively used as a working electrode and a counter electrode, are immersed into a container containing trifluoroacetic acid aqueous solution with the concentration of 3mmol/L, and then the two ends of the clamp are respectively connected with the positive electrode and the negative electrode of a direct current power supply.
(4) The film was deposited using a voltage of 30V for 60 minutes.
(5) The prepared film is annealed for 60 minutes at 800 ℃ under the protection of nitrogen. And then cooling to room temperature under the protection of gas to obtain a C film.
Performing microstructure characterization on the film by using a transmission electron microscope and a Raman spectrometer, wherein the microstructure characterization is respectively shown in figures 1 and 2; the composition of the film was characterized by photoelectron spectroscopy as shown in FIG. 3. As can be seen from fig. 1, the prepared film has an onion structure; typical D and G peaks shown in fig. 2, illustrate that the films produced are indeed carbon films; FIG. 3 shows that the carbonyl group in the organic molecular film has decomposed and the film contains fluorine.
A friction tester is utilized, a steel ball is used as a friction matching pair, a friction experiment is carried out under the conditions that the load is 0.05N, the linear speed is 0.02m/s, and the testing time is 30min, and the tribological performance of the film is inspected by a three-dimensional surface profiler.
[ example 4 ]
(1) An N-type polished monocrystalline silicon wafer with a crystal orientation of < 100 > and a resistivity of 0.01 omega-m was cut into two small silicon wafers of 1cm × 2cm size with a diamond knife.
(2) The silicon wafer of the above size was put in a chamber containing 98% H in a volume ratio of 7:32SO4And 30% H2O2And cleaning the silicon wafer in a wide-mouth bottle of the mixed solution by using an ultrasonic cleaner, then cleaning the silicon wafer for several times by using ultrapure water, and finally drying the silicon wafer by using nitrogen.
(3) Two silicon wafers are clamped by a clamp, are arranged in parallel face to face at a distance of 5mm, are respectively used as a working electrode and a counter electrode, are immersed into a container containing trifluoroacetic acid aqueous solution with the concentration of 3mmol/L, and then the two ends of the clamp are respectively connected with the positive electrode and the negative electrode of a direct current power supply.
(4) A voltage of 35V was used to deposit the film for 60 minutes.
(5) And annealing the prepared film at 800 ℃ for 60 minutes under the protection of argon. And then cooling to room temperature under the protection of gas to obtain a D film.
A friction tester is utilized, a steel ball is used as a friction matching pair, a friction experiment is carried out under the conditions that the load is 0.05N, the linear speed is 0.02m/s, and the testing time is 30min, and the tribological performance of the film is inspected by a three-dimensional surface profiler.
TABLE 1
| Examples | 1 | 2 | 3 | 4 |
| Coefficient of friction | 0.0343 | 0.0437 | 0.0303 | 0.0330 |
| Wear rate (10)-4mm3/Nm) | 1.4491 | 1.4388 | 1.2600 | 1.6061 |
Table 1 shows the friction coefficient and wear rate data for A, B, C and D four fluorine-containing onion carbon films prepared in examples 1, 2, 3, and 4, with overall friction coefficients between 0.03 and 0.04. The invention improves tribological performance by doping the onion carbon with fluorine.
Compared with the friction coefficient (0.04-0.08) of the onion carbon film prepared in the invention patent application with the application number of CN201711361086, the friction coefficient is reduced by about one fourth. Also, as can be seen from Table 1, of the four fluorine-containing onion carbon films, the C film prepared in example 3 had a friction coefficient (0.0303) and a wear rate (1.2600X 10)-4mm3/Nm), namely the film C has the most excellent friction-reducing and wear-resisting properties.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (10)
1. The method for directly preparing the low-friction fluorine-containing onion carbon film on the silicon substrate is characterized in that the molecular film deposited by the annealing electrophoresis method is directly used for preparing the low-friction fluorine-containing onion carbon on the silicon substrate, and the method comprises the following steps:
(1) using 98% H with volume ratio of 7:32SO4And 30% H2O2Cleaning the silicon wafer by using the mixed solution, then cleaning the silicon wafer for several times by using ultrapure water, and finally drying the silicon wafer by using nitrogen;
(2) placing two silicon wafers in parallel face to face, immersing the two silicon wafers into an organic monocarboxylic acid aqueous solution to be used as a working electrode and a counter electrode respectively, and then connecting two ends of the two silicon wafers with the positive electrode and the negative electrode of a direct current power supply respectively;
(3) electrifying a working electrode and a counter electrode, and depositing an organic monocarboxylic acid film on the surface of a silicon wafer by adopting an electrophoresis method;
(4) and (3) annealing the prepared organic monocarboxylic acid film under the protection of inert gas, decomposing the organic monocarboxylic acid, and allowing carbonyl groups to escape in the form of carbon dioxide and water, wherein the obtained film is a carbon film with an onion structure and contains fluorine.
2. The method for preparing a low-friction fluorine-containing onion carbon film directly on a silicon substrate as claimed in claim 1, wherein the silicon wafer used is an N-type polished single crystal silicon wafer having a crystal orientation of < 100 > and a resistivity of 0.001 to 1.5 Ω -m.
3. The method for preparing a low-friction fluorine-containing onion carbon film directly on a silicon substrate as claimed in claim 1, wherein a distance between two silicon wafers as a working electrode and a counter electrode is 2 to 20 mm.
4. The method of claim 1, wherein the organic monocarboxylic acid is one of trifluoroacetic acid, trifluoropropionic acid, heptafluorobutyric acid, pivalic acid, undecafluorohexanoic acid, perfluoroheptanoic acid.
5. The method of claim 1, wherein the concentration of the aqueous solution of organic monocarboxylic acid is 0.5 to 10 mmol/L.
6. The method of claim 1, wherein the voltage during the electrophoretic deposition of the thin film is 5-50V.
7. The method of claim 1, wherein the electrophoretic deposition time for depositing the film is 10-120 min.
8. The method for preparing a low-friction fluorine-containing onion carbon film directly on a silicon substrate as claimed in claim 1, wherein the inert shielding gas is one or more of nitrogen, argon and helium.
9. The method as claimed in claim 1, wherein the annealing temperature of the film is 300-900 ℃ and the holding time is 30-120 min.
10. The low-friction fluorine-containing onion carbon film produced by the method for producing a low-friction fluorine-containing onion carbon film according to any one of claims 1 to 9, wherein the carbon film produced has an onion structure and contains fluorine.
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| WO2015116007A1 (en) * | 2014-01-30 | 2015-08-06 | The Thailand Research Fund | Catalytic carbon counter electrode for dye-sensitized solar cells |
| CN105506716A (en) * | 2015-12-25 | 2016-04-20 | 苏州宏久航空防热材料科技有限公司 | Preparation method for high-bonding wearproof composite coating |
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| WO2015116007A1 (en) * | 2014-01-30 | 2015-08-06 | The Thailand Research Fund | Catalytic carbon counter electrode for dye-sensitized solar cells |
| JP2016096810A (en) * | 2014-11-26 | 2016-05-30 | 株式会社マツモト | Machine for peeling vegetables |
| CN105506716A (en) * | 2015-12-25 | 2016-04-20 | 苏州宏久航空防热材料科技有限公司 | Preparation method for high-bonding wearproof composite coating |
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