CN103333536A - Application of monoatomic layer boron nitride in surface coating - Google Patents
Application of monoatomic layer boron nitride in surface coating Download PDFInfo
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- CN103333536A CN103333536A CN2013102225715A CN201310222571A CN103333536A CN 103333536 A CN103333536 A CN 103333536A CN 2013102225715 A CN2013102225715 A CN 2013102225715A CN 201310222571 A CN201310222571 A CN 201310222571A CN 103333536 A CN103333536 A CN 103333536A
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Abstract
The invention provides application of monoatomic layer boron nitride in a surface coating. An applicable substrate comprises metal or semiconductor with an insulated oxide layer or an insulated dielectric layer, or is a high polymer flexible material or a non-conductive inorganic material or conductive metal or a photosensitive semiconductor material. The surface of the substrate can be flat or bent. The preparation method of a boron nitride film layer comprises the following steps of: chemical vapor deposition, epitaxial growth, plasma sputtering and magnetron sputtering. The way for bonding boron nitride comprises directly growing or transferring to the surface of the substrate. under the condition that the thickness and appearance of the substrate of the coating are hardly changed, the wettability of the substrate can be directly converted into the wettability of boron nitride, and the anti-friction performance and anti-oxidation performance of the substrate are enhanced.
Description
Technical field
The present invention relates to field of surface coatings, specifically is the application of a kind of monoatomic layer boron nitride in top coat.
Background technology
Solid surface coating and adjustability thereof have important use in fields such as biology, agricultural, oil, agricultural chemicals, electronics.The method that changes nature of solid surface is a lot, mainly comprise change solid surface pattern, electric wetting adjusting, be coated with organic polymer or inorganics etc. at solid surface, but these methods have often changed the surface topography of solid, and thickness etc. have limited these methods and used in some environment.
Hexagonal boron nitride is a kind of monoatomic layer structure of broad stopband isolator of the 5.97eV of having direct band gap, has good mechanics, optical property, remarkable thermostability and chemical stability, can stable existence to 1000 in the oxygen environment ℃ more than.And individual layer boron nitride thickness 0.33 nm that only has an appointment, it does not absorb in the visible-range interior focusing simultaneously, only there is a little light to absorb in the ultraviolet region, it covers thickness and exterior appearance that solid surface can not change solid, but the anti-oxidant friction resistant character that can effectively change, can also change simultaneously the wettability of solid surface, be widely used in the heatshield material in high temperature solid lubricant, the space flight and aviation, the fields such as spout of aircraft rocket motor, but in field of surface coatings application do not arranged as yet.
Summary of the invention
The invention provides the application of monoatomic layer boron nitride in top coat and the growth method of this coating, under the situation of the thickness that changes substrate hardly and outward appearance, directly the wettability of substrate is converted into the wettability of boron nitride itself, friction resistant performance and the antioxidant property of enhancing substrate.
The invention provides the application of a kind of monoatomic layer boron nitride in top coat.
Further improve, the substrate of using monoatomic layer boron nitride top coat comprises metal or the semi-conductor that has insulating oxide or insulation dielectric layer, or the polymer flexible materials, or nonconducting inorganic materials, or the metal of conduction, or light-sensitive semiconductor material.
Further improve, described substrate surface is smooth or crooked.
Further improve, the preparation method of boron nitride top coat comprises chemical Vapor deposition process, epitaxial growth method, plasma sputtering, magnetron sputtering method.
Further improving, is to be transferred to substrate surface after direct growth or the growth in conjunction with the mode of boron nitride.
Beneficial effect of the present invention is: on the basis of the thickness that can change substrate hardly and exterior appearance, can directly the wettability of substrate be converted into the wettability of boron nitride itself, strengthen friction resistant performance and the antioxidant property of substrate simultaneously, and have erosion resistance preferably.
Description of drawings
Fig. 1 is the sign to boron nitride: wherein, and (a) for transferring to SiO
2The optical photograph of the suprabasil boron nitride of/Si is the light transmission spectrum of boron nitride (b), (c) is transmission electron microscope photo, (d) is selected area electron diffraction.
The frictional force comparison diagram that have or not copper substrate that boron nitride cover of Fig. 2 for measuring among the embodiment 1.
The optical photograph comparison diagram of the copper substrate that has or not the boron nitride covering of heating under 200 oC in air that Fig. 3 (a) measures for embodiment 2 (b) is energy dispersion X ray spectral signal comparison diagram.
The contact angle comparison diagram that have or not various substrates that boron nitride cover of Fig. 4 for measuring among the embodiment 2.
The contact angle comparison diagram of the titanium dioxide substrate that under the irradiation of ultraviolet lamp, has or not the boron nitride covering that Fig. 5 measures for embodiment 3.
Embodiment
The applicable substrate of the present invention comprises metal or the semi-conductor that has insulating oxide or insulation dielectric layer, or the polymer flexible materials, or nonconducting inorganic materials, or the metal of conduction, or light-sensitive semiconductor material.
Substrate surface can be smooth or crooked.
The preparation method of boron nitride rete comprises chemical Vapor deposition process, epitaxial growth method, plasma sputtering, magnetron sputtering method.
Can be to be transferred to substrate surface after direct growth or the growth in conjunction with the mode of boron nitride.If substrate is metallic substance, but transfer in the substrate after boron nitride rete direct growth or the growth; If substrate is non-metallic material, the boron nitride rete can only be transferred on the non metallic substrate after the metal base growth again.
The method of monoatomic layer boron nitride top coat direct growth may further comprise the steps:
1) will put into reaction chamber behind the metal base cleaning, drying;
2) will be as the ammonia borane complex compound reaction source preheating of boron, nitrogenous source with 50-200 ℃ temperature;
3) growth temperature of keeping reaction chamber is 900-1100 ℃, and the ammonia borane complex compound reaction source after the preheating is imported reaction chamber and feeds hydrogen with 5-15sccm simultaneously with gaseous state, grows after 10-20 minute, closes the ammonia borane source;
4) under the protection of 5-15sccm hydrogen gas stream, be cooled fast to room temperature, obtain the boron nitride pellicle that the number of plies is the 1-2 layer in substrate.
The method that shift monoatomic layer boron nitride top coat growth back may further comprise the steps:
1) will put into reaction chamber behind the copper sheet cleaning, drying;
2) will be as the ammonia borane complex compound reaction source preheating of boron, nitrogenous source with 50-200 ℃ temperature;
3) growth temperature of keeping reaction chamber is 900-1100 ℃, and the ammonia borane complex compound reaction source after the preheating is imported reaction chamber and feeds hydrogen with 5-15sccm simultaneously with gaseous state, grows after 10-20 minute, closes the ammonia borane source;
4) under the protection of 5-15sccm hydrogen gas stream, be cooled fast to room temperature, obtain the boron nitride pellicle that the number of plies is the 1-2 layer at copper sheet;
5) the copper sheet surface that will be coated with boron nitride is coated with polymetylmethacrylate solution, after the solvent evaporates copper sheet is placed the ferric chloride Solution of 0.1M to soak more than 24 hours, treat that copper dissolves fully after, obtain floating on the boron nitride-PMMA layer on the solution;
6) boron nitride-PMMA layer is transferred in the substrate, after firmly, repeatedly cleaned with dilute hydrochloric acid, deionized water successively, then with a large amount of acetone solution PMMA, can obtain monoatomic layer boron nitride top coat at substrate surface.
Below in conjunction with the drawings and specific embodiments the present invention is elaborated, but the present invention is not limited to following example.
Method described in the following embodiment if no special instructions, is ordinary method; Described reagent and material etc. if no special instructions, all can obtain from commercial channels.
Embodiment 1
Be substrate with 25 micron thickness Copper Foils, will be as the ammonia borane complex compound reaction source preheating of boron, nitrogenous source under 50 ℃ temperature; What keep reaction chamber is 900 ℃ in growth temperature, and the ammonia borane complex compound reaction source after the preheating is imported reaction chamber and feeds hydrogen with 10sccm simultaneously with gaseous state, grows after 20 minutes, closes the ammonia borane source; Under the protection of 10sccm hydrogen gas stream, be cooled fast to room temperature, obtain the boron nitride pellicle that the number of plies is the 1-2 layer at matrix;
With atomic force microscope friction measurement pattern after to simple annealing the naked copper substrate and the copper substrate behind the growing boron nitride carry out friction measurement.Measuring result is seen Fig. 2, and the frictional force that has covered the copper substrate of individual layer boron nitride coating has reduced more than 40 times than the frictional force of naked copper.
Carry out with naked copper substrate and the copper substrate behind the growing boron nitride of warm table after to simple annealing that 200oC heats in air, detect its antioxidation property.Measuring result is seen Fig. 3, and after the copper substrate that has covered the individual layer boron nitride coating was heated in air, its color did not change, and the surface does not detect the existence of Sauerstoffatom yet.And after naked copper heated in air, very big variation had taken place in color, and the surface has detected the existence of Sauerstoffatom.
Embodiment 2
Be substrate with 20 micron thickness nickel foils, will be as the ammonia borane complex compound reaction source preheating of boron, nitrogenous source under 100 ℃ temperature; What keep reaction chamber is 1000 ℃ in growth temperature, and the ammonia borane complex compound reaction source after the preheating is imported reaction chamber and feeds hydrogen with 15sccm simultaneously with gaseous state, grows after 5 minutes, closes the ammonia borane source; Under the protection of 15sccm hydrogen gas stream, be cooled fast to room temperature, obtain the boron nitride pellicle that the number of plies is the 1-2 layer at matrix;
Prepare quartz substrate: used acetone, ethanol, deionized water ultrasonic cleaning quartz substrate successively respectively 10 minutes, oven dry then.
The copper sheet surface that is coated with boron nitride is coated with PMMA solution, place the 1M hydrochloric acid soln to soak the nickel sheet after the solvent evaporates, after 24 hours, copper dissolves fully, obtain floating on the boron nitride-PMMA layer on the solution, it is transferred on the quartz substrate, after firmly, repeatedly clean with dilute hydrochloric acid, deionized water successively, with a large amount of acetone solution PMMA, obtain transferring to the boron nitride layer structure on the quartz substrate then.
Fig. 1 is the various signs to boron nitride, can see that the boron nitride that obtains is individual layer, and clean performance is good, and intact the transferring in the substrate of energy almost do not have breakage.
Transfer to the photoabsorption of silica based individual layer boron nitride on the ground with the measurement of measurement of ultraviolet-visible spectrophotometer instrument, the results are shown in Figure 1(b), visible boron nitride does not have photoabsorption at visible region, and a spot of photoabsorption is only arranged in ultraviolet region.
Respectively the quartz substrate after simple quartz substrate and the transfer boron nitride being carried out contact angle with contact angle measurement measures.Fig. 4 has or not the contact angle comparison diagram that covers boron nitride for various substrates.
Embodiment 3
Be substrate with 30 micron thickness Copper Foils, will be as the ammonia borane complex compound reaction source preheating of boron, nitrogenous source under 200 ℃ temperature; What keep reaction chamber is 1100 ℃ in growth temperature, and the ammonia borane complex compound reaction source after the preheating is imported reaction chamber and feeds hydrogen with 5sccm simultaneously with gaseous state, grows after 20 minutes, closes the ammonia borane source; Under the protection of 5sccm hydrogen gas stream, be cooled fast to room temperature, obtain the boron nitride pellicle that the number of plies is the 1-2 layer at matrix;
Prepare the titanium dioxide substrate: used acetone, ethanol, deionized water ultrasonic cleaning quartz substrate successively respectively 10 minutes, oven dry then.
The copper sheet surface that is coated with boron nitride is coated with PMMA solution, place the 0.1M ferric chloride Solution to soak copper sheet after the solvent evaporates, after 24 hours, copper dissolves fully, obtain floating on the boron nitride-PMMA layer on the solution, it is transferred in the titanium dioxide substrate, after firmly, repeatedly clean with dilute hydrochloric acid, deionized water successively, with a large amount of acetone solution PMMA, obtain transferring to the boron nitride layer structure in the titanium dioxide substrate then.
Respectively contact angle being carried out in the titanium dioxide substrate after simple titanium dioxide substrate and the transfer boron nitride with contact angle measurement measures.To have or not the titanium dioxide substrate of boron nitride to be put into irradiation 10 min under the ultraviolet lamp respectively, and carry out contact angle with contact angle measurement then and measure.Be put under the ultraviolet lamp irradiation 10 min again, carry out contact angle with contact angle measurement then and measure.Measuring result is seen Fig. 5, and the contact angle of titanium dioxide substrate changes along with the variation of irradiation time, but the contact angle that has covered the substrate of boron nitride remains unchanged.
The concrete application approach of the present invention is a lot, and the above only is preferred implementation of the present invention, should be understood that; for those skilled in the art; under the prerequisite that does not break away from the principle of the invention, can also make some improvement, these improvement also should be considered as protection scope of the present invention.
Claims (5)
1. the application of monoatomic layer boron nitride in top coat.
2. the application of monoatomic layer boron nitride according to claim 1 in top coat, it is characterized in that: the substrate of using monoatomic layer boron nitride top coat comprises metal or the semi-conductor that has insulating oxide or insulation dielectric layer, or polymer flexible materials, or nonconducting inorganic materials, or the metal of conduction, or light-sensitive semiconductor material.
3. the application of monoatomic layer boron nitride according to claim 2 in top coat is characterized in that: described substrate surface is smooth or crooked.
4. the application of monoatomic layer boron nitride according to claim 1 in top coat, it is characterized in that: the preparation method of boron nitride top coat comprises chemical Vapor deposition process, epitaxial growth method, plasma sputtering, magnetron sputtering method.
5. according to the application of the above described monoatomic layer boron nitride of any claim in top coat, it is characterized in that: be to be transferred to substrate surface after direct growth or the growth in conjunction with the mode of boron nitride.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104532209A (en) * | 2015-01-27 | 2015-04-22 | 厦门大学 | Method for preparing wafer-grade large-size hexagonal boron nitride on substrate |
| CN108489298A (en) * | 2018-04-19 | 2018-09-04 | 浙江大学 | The plasma coal pyrolysis quenching device of included boron nitride coating protection anti-wear cover |
| CN109411115A (en) * | 2018-09-04 | 2019-03-01 | 苏州泰吉诺新材料科技有限公司 | A kind of high torque heat-conduction insulation spacer material and its production technology |
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| CN1389910A (en) * | 2001-05-31 | 2003-01-08 | 三星电子株式会社 | Method for forming film using atomic layer deposition |
| CN102173406A (en) * | 2010-12-24 | 2011-09-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method for carbon nano tube or graphene extra-thin film |
| CN103663416A (en) * | 2012-09-01 | 2014-03-26 | 董国材 | Method for preparing graphene and single-layer hexagonal boron nitride composite material |
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- 2013-06-06 CN CN2013102225715A patent/CN103333536A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1389910A (en) * | 2001-05-31 | 2003-01-08 | 三星电子株式会社 | Method for forming film using atomic layer deposition |
| CN102173406A (en) * | 2010-12-24 | 2011-09-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method for carbon nano tube or graphene extra-thin film |
| CN103663416A (en) * | 2012-09-01 | 2014-03-26 | 董国材 | Method for preparing graphene and single-layer hexagonal boron nitride composite material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104532209A (en) * | 2015-01-27 | 2015-04-22 | 厦门大学 | Method for preparing wafer-grade large-size hexagonal boron nitride on substrate |
| CN104532209B (en) * | 2015-01-27 | 2017-12-29 | 厦门大学 | A kind of method that wafer scale large scale hexagonal boron nitride is prepared in substrate |
| CN108489298A (en) * | 2018-04-19 | 2018-09-04 | 浙江大学 | The plasma coal pyrolysis quenching device of included boron nitride coating protection anti-wear cover |
| CN109411115A (en) * | 2018-09-04 | 2019-03-01 | 苏州泰吉诺新材料科技有限公司 | A kind of high torque heat-conduction insulation spacer material and its production technology |
| CN109411115B (en) * | 2018-09-04 | 2020-02-28 | 苏州泰吉诺新材料科技有限公司 | High-torque heat-conducting insulating gasket material and production process thereof |
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Application publication date: 20131002 |