CN111005010A - Preparation method, product and application of nano-diamond metallized film - Google Patents
Preparation method, product and application of nano-diamond metallized film Download PDFInfo
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- CN111005010A CN111005010A CN201911310594.5A CN201911310594A CN111005010A CN 111005010 A CN111005010 A CN 111005010A CN 201911310594 A CN201911310594 A CN 201911310594A CN 111005010 A CN111005010 A CN 111005010A
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- 239000002113 nanodiamond Substances 0.000 title claims abstract description 41
- 239000011104 metalized film Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000010408 film Substances 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 31
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 30
- 239000010432 diamond Substances 0.000 claims abstract description 30
- 238000003486 chemical etching Methods 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims abstract description 5
- 229910044991 metal oxide Inorganic materials 0.000 claims description 17
- 150000004706 metal oxides Chemical class 0.000 claims description 17
- 238000004528 spin coating Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001020 plasma etching Methods 0.000 claims description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 2
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 2
- 239000000758 substrate Substances 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- 238000012805 post-processing Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 24
- 238000002156 mixing Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 6
- 239000000084 colloidal system Substances 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 229910003481 amorphous carbon Inorganic materials 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000002431 foraging effect Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001465 metallisation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- YZCKVEUIGOORGS-UHFFFAOYSA-N Hydrogen atom Chemical compound [H] YZCKVEUIGOORGS-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 229910021386 carbon form Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
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- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
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Abstract
本发明公开一种纳米金刚石金属化薄膜的制备方法、产品及应用，具体通过以下方法制备得到：采用化学刻蚀的方法，在硅衬底上制备多孔金刚石薄膜；将制备得到金刚石薄膜与金属氧化物的凝胶，均匀旋涂，形成致密薄膜，干燥，制得多孔纳米金刚石/氧化物复合薄膜，本发明针对纳米金刚石薄膜形成多孔结构之后造成的导电性与活性位点的下降问题，对纳米金刚石薄膜进行合理的后期处理，有效地得到了金属化的多孔纳米金刚石薄膜材料。
The invention discloses a preparation method, product and application of a nano-diamond metallized film, which are specifically prepared by the following methods: using a chemical etching method to prepare a porous diamond film on a silicon substrate; The gel of the material is uniformly spin-coated to form a dense film, and dried to obtain a porous nano-diamond/oxide composite film. After reasonable post-processing of the diamond film, the metallized porous nano-diamond film material is effectively obtained.
Description
Technical Field
The invention relates to the technical field of diamond films, in particular to a preparation method, a product and application of a nano-diamond metallized film.
Background
The nano diamond film is a film nano diamond material deposited on the surface of a substrate by utilizing various vapor deposition methods, consists of nano diamond grains and amorphous carbon grain boundaries, and is widely applied to the aspects of bioelectrode, chemical sewage treatment and the like due to the characteristics of high hardness, high thermal conductivity, acid and alkali resistance, chemical stability and the like of diamond. The preparation method is that carbon compound and hydrogen are used as main raw materials, a diamond film is generated on the surface of a substrate by using a chemical vapor deposition technology at low temperature and low pressure, the former provides a carbon source, the latter provides atomic hydrogen, more carbon is promoted to be converted into a sp3 diamond structure, and other carbon forms (sp2 graphite carbon or amorphous carbon, sp1 carbon) which are not converted into diamond are removed. However, in the chemical vapor deposition process, the problem that the diamond film generates a large amount of amorphous carbon to be filled in the grain boundary position due to the mismatching of the raw material gas proportion often exists, so that the performance of the nano-diamond film is greatly influenced. However, the removal of the amorphous carbon film also causes the decrease of the conductivity or the number of catalytically active sites of the film, so how to further increase the conductivity or the number of catalytically active sites of the nano-diamond film becomes a technical problem to be solved by those skilled in the art.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method, a product and an application of nano-diamond metallization, wherein a porous nano-diamond film is subjected to metallization treatment, so that the conductive property of the film is improved, and the sites with chemical reaction activity can be increased, so that the film material can be better applied to the fields of nano-diamond electrical device manufacturing and bioelectrode detection.
One of the technical schemes of the invention is a method for preparing a nano-diamond metallized film, which comprises the following steps,
step (1): preparing a porous diamond film from the diamond film by adopting a chemical etching method;
step (2): uniformly spin-coating a gel solution of a metal oxide on the surface of the porous diamond film prepared in the step (1) to form a compact film, and drying to prepare a porous nano diamond/oxide composite film;
and (3): and (3) carrying out plasma etching treatment on the porous nano-diamond/oxide composite film prepared in the step (2) by adopting a microwave plasma method to obtain the nano-diamond metallized film.
Preferably, the chemical etching method in the step (1) is to soak the diamond film in a concentrated sulfuric acid solution, take out and dry the diamond film to obtain the porous diamond film, wherein the concentrated sulfuric acid solution has a volume fraction of 75%, the soaking time is 20-60min, and the drying condition is vacuum drying at 200 ℃.
Preferably, the preparation method of the metal oxide gel in the step (2) is a gel method
Preferably, the metal oxide is one of nickel oxide, titanium oxide, and tungsten oxide.
Preferably, the thickness of the spin coating in the step (2) is 1-15 um.
Preferably, the drying condition in step (2) is 100-200 ℃ vacuum drying.
Preferably, the microwave plasma etching method is specifically microwave power of 1000-2The concentration is 20-200sccm, and the etching time is 30-60 min.
According to the second technical scheme, the nano-diamond metallized film is prepared by the preparation method of the nano-diamond metallized film.
In the third technical scheme of the invention, the nano-diamond metalized film is applied to the manufacturing of nano-diamond electrical devices and the detection of bioelectrode.
Compared with the prior art, the invention has the following beneficial effects:
(1) the porous diamond/metal oxide colloid film is subjected to plasma etching treatment, so that oxygen elements in the oxide deposited in a pore structure escape under the action of H ions, oxygen in the oxide gathered in a nano-diamond grain boundary is selectively removed, a uniform metal layer is formed in the porous structure, and the metal-filled nano-diamond grain structure film is formed, so that the binding force between metal particles and diamond grains is improved, and the formation of the metal layer improves the conductive property of the film on one hand and can increase sites with chemical reaction activity on the other hand;
(2) the plasma etching method enables oxygen elements on the surface of the oxide to rapidly escape under the action of H plasma, so that an oxygen vacancy structure is formed, a convex-concave surface is formed during excessive etching, and the surface of the material is greatly changed, so that the surface structure of the film is improved, and the surface adsorption performance of the film as an electrode is improved.
Drawings
Fig. 1 is an SEM image of a nanodiamond metallized film prepared in example 1 of the invention.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
The preparation of the metal oxide gel can be carried out by a gel method in the prior art, and preferably, the preparation method of the metal oxide gel comprises the following steps: weighing metal oxide, ethanol and water in a molar ratio of 1: 1-50, uniformly mixing the metal oxide and part of ethanol to form a solution A, uniformly mixing water and the rest of ethanol to form a solution B, adjusting the pH value to 1-4, dropwise adding the solution A into the solution B, stirring, standing for aging after dropwise adding is completed, and finally obtaining the metal oxide gel.
Example 1
Preparation of titanium oxide gel, butyl titanate: ethanol: the molar ratio of water is 1: 18: 40.
firstly, mixing butyl titanate with half of ethanol to form a solution A; mixing water with the other half of ethanol to form a solution B, and adjusting the pH value of the solution B to 2 by using nitric acid; and dropwise adding the solution A into the solution B, stirring, and standing for aging after dropwise adding is completed to finally obtain the titanium oxide gel.
Soaking a 25-micron nano-diamond film in a 75% concentrated sulfuric acid solution for 30min, taking out and drying to obtain a porous diamond film, taking a silicon substrate as a substrate for preparing the nano-diamond metallized film, spin-coating a metal oxide colloid solution on the porous diamond film in a spin-coating mode, spin-coating the metal oxide colloid solution to a thickness of 10 mu m, and drying to form a film under the vacuum environment condition of 150 ℃. And (3) carrying out plasma etching treatment on the film by adopting a microwave plasma method, wherein the microwave power is 1000W, hydrogen is used as reducing gas, the concentration is 50sccm, the oxide in the porous film is subjected to reducing etching, and the etching time is 1 hour, so that the porous diamond metallized film with the thickness of 34um is prepared.
Example 2
Preparation of titanium oxide gel, butyl titanate: ethanol: the molar ratio of water is 1: 18: 20.
firstly, mixing butyl titanate with half of ethanol to form a solution A; mixing water with the other half of ethanol to form a solution B, and adjusting the pH value of the solution B to 3.5 by using nitric acid; and dropwise adding the solution A into the solution B, stirring, and standing for aging after dropwise adding is completed to finally obtain the titanium oxide gel.
Soaking the 20 mu m nano-diamond film in 75% concentrated sulfuric acid solution for 30min, fishing up and drying to obtain a porous diamond film, taking a silicon substrate as a substrate for preparing the nano-diamond metallized film, spin-coating a metal oxide colloid solution onto the porous diamond film in a spin-coating mode, wherein the spin-coating thickness is 3 mu m, and drying to form a film under the vacuum environment condition of 200 ℃. And (3) carrying out plasma etching treatment on the film by adopting a microwave plasma method, wherein the microwave power is 1200W, hydrogen is used as reducing gas, the concentration is 100sccm, the oxide in the porous film is subjected to reducing etching, the etching time is 0.5 hour, and the prepared thickness is 22 um.
Example 3
Preparation of titanium oxide gel, butyl titanate: ethanol: the molar ratio of water is 1: 15: 20.
firstly, mixing butyl titanate with half of ethanol to form a solution A; mixing water with the other half of ethanol to form a solution B, and adjusting the pH value of the solution B to 3.5 by using nitric acid; and dropwise adding the solution A into the solution B, stirring, and standing for aging after dropwise adding is completed to finally obtain the titanium oxide gel.
Soaking a 30-micron nano-diamond film in a 75% concentrated sulfuric acid solution for 30min, fishing out and drying to obtain a porous diamond film, taking a silicon substrate as a substrate for preparing the nano-diamond metallized film, spin-coating a metal oxide colloid solution on the porous diamond film in a spin-coating mode, spin-coating the metal oxide colloid solution to a thickness of 5 mu m, and drying to form a film under the vacuum environment condition of 150 ℃. And (3) carrying out plasma etching treatment on the film by adopting a microwave plasma method, wherein the microwave power is 1500W, hydrogen is taken as reducing gas, the concentration is 150sccm, the oxide in the porous film is subjected to reducing etching, the etching time is 1 hour, and the porous diamond metallized film with the thickness of 33um is prepared.
Claims (9)
1. A method for preparing a nano-diamond metallized film is characterized by comprising the following steps,
step (1): preparing a porous diamond film from the diamond film by adopting a chemical etching method;
step (2): uniformly spin-coating the gel solution of the metal oxide on the surface of the porous diamond film prepared in the step (1) to form a compact film, and drying to prepare a porous nano diamond/oxide composite film;
and (3): and (3) carrying out plasma etching treatment on the porous nano-diamond/oxide composite film prepared in the step (2) by adopting a microwave plasma method to obtain the nano-diamond metallized film.
2. The method for preparing a nano-diamond metallized film according to claim 1, wherein the chemical etching method in step (1) is to soak the diamond film in a concentrated sulfuric acid solution, then take out and dry the diamond film to obtain the porous diamond film, wherein the volume fraction of the concentrated sulfuric acid solution is 75%, the soaking time is 20-60min, and the drying condition is 100-200 ℃ vacuum drying.
3. The method of claim 1, wherein the metal oxide gel of step (2) is prepared by a gel process.
4. The method of claim 1, wherein the metal oxide is one of nickel oxide, titanium oxide, and tungsten oxide.
5. The method of claim 1, wherein the spin-coating thickness in step (2) is 1-15 um.
6. The method for preparing a nano-diamond metallized film according to claim 1, wherein the drying condition of step (2) is 100-200 ℃ vacuum drying.
7. The method as claimed in claim 1, wherein the microwave plasma method is selected from the group consisting of microwave power 1000-2The concentration is 20-200sccm, and the etching time is 30-60 min.
8. A nanodiamond metallized film produced by the method of producing a nanodiamond metallized film according to any one of claims 1-7.
9. Use of the nanodiamond metallized film of claim 8 in the fabrication of nanodiamond electrical devices and bioelectrode probing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113186510A (en) * | 2021-04-28 | 2021-07-30 | 昆明理工大学 | Metal reinforced porous diamond film and preparation method thereof |
| CN113755813A (en) * | 2021-09-10 | 2021-12-07 | 安徽光智科技有限公司 | Substrate pretreatment method and diamond film preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113186510A (en) * | 2021-04-28 | 2021-07-30 | 昆明理工大学 | Metal reinforced porous diamond film and preparation method thereof |
| CN113755813A (en) * | 2021-09-10 | 2021-12-07 | 安徽光智科技有限公司 | Substrate pretreatment method and diamond film preparation method |
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| CN111005010B (en) | 2021-05-25 |
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