CN113088849A - Composite strengthening method for synthesizing nano diamond by laser induction - Google Patents
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- 238000005728 strengthening Methods 0.000 title claims abstract description 42
- 239000002113 nanodiamond Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 230000006698 induction Effects 0.000 title claims description 9
- 230000002194 synthesizing effect Effects 0.000 title claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 15
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 14
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 13
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 8
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 8
- 230000035939 shock Effects 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 8
- 239000004065 semiconductor Substances 0.000 claims description 7
- 230000009471 action Effects 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 238000003618 dip coating Methods 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 230000001680 brushing effect Effects 0.000 claims 1
- 239000010432 diamond Substances 0.000 abstract description 35
- 229910003460 diamond Inorganic materials 0.000 abstract description 35
- 239000000463 material Substances 0.000 abstract description 19
- 239000002245 particle Substances 0.000 abstract description 18
- 239000013078 crystal Substances 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 239000010949 copper Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 229920001721 polyimide Polymers 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000004100 electronic packaging Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
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- 239000007777 multifunctional material Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- C01B32/26—Preparation
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- Condensed Matter Physics & Semiconductors (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
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Abstract
本发明公开了一种激光诱导合成纳米金刚石的复合强化方法，步骤如下：(1)在构件的表面均匀涂覆碳源，借助二氧化碳激光器发射激光束并连续辐照碳源表面，将其转化为石墨烯或活性炭层；(2)在碳层上方铺设约束层；(3)采用飞秒激光器发射脉冲激光束，并采用加热激光器发射连续激光束，保证两束激光光斑中心重合且辐照于碳层表面；(4)将三维数控移动平台或者激光器至下一强化位置开展激光冲击复合强化作业。本发明可在易损构件外表面诱导生成纳米金刚石颗粒，形成压缩应力层，实现高硬度金刚石的直接强化，同时细化构件表面晶粒，并产生沿厚度方向梯度分布的晶粒组织，能够在不牺牲材料延展性的同时，有效提升材料的强度。
The invention discloses a composite strengthening method for laser-induced synthesis of nano-diamonds. The steps are as follows: (1) uniformly coat a carbon source on the surface of a component, emit a laser beam by means of a carbon dioxide laser and continuously irradiate the surface of the carbon source, and convert it into Graphene or activated carbon layer; (2) Laying a constraining layer on top of the carbon layer; (3) Using a femtosecond laser to emit a pulsed laser beam, and a heating laser to emit a continuous laser beam, to ensure that the centers of the two laser spots overlap and irradiate on the carbon (4) The three-dimensional numerical control mobile platform or the laser is moved to the next strengthening position to carry out the laser shock composite strengthening operation. The invention can induce the formation of nano-diamond particles on the outer surface of the vulnerable component, form a compressive stress layer, realize the direct strengthening of high-hardness diamond, and at the same time refine the crystal grains on the surface of the component, and generate a grain structure with a gradient distribution along the thickness direction. Effectively improve the strength of the material without sacrificing the ductility of the material.
Description
Technical Field
The invention relates to the technical field of material surface modification, in particular to a composite strengthening method for synthesizing nano-diamond by laser induction.
Background
The nano-diamond is a multifunctional material, is widely applied to the fields of biosensors, quantum computing, fuel cells, computer chips and the like because of excellent thermodynamic properties, and can obviously improve the comprehensive mechanical properties of metal base materials as a dispersion strengthening phase of a composite material. In engineering, the nano-diamond can be directly or indirectly applied to surface strengthening of a vulnerable component to improve the strength and the tribological performance of the component, for example, Wang Wentang et Al (publication number: CN101728279A) propose a preparation method of a high-performance diamond-strengthened Al-based electronic packaging composite material, and an electronic packaging material with excellent comprehensive mechanical properties can be obtained by adding single-crystal diamond particles and compositing the single-crystal diamond particles with high-thermal-conductivity metal Al, but the process flow of the diamond strengthening mechanism is complicated, and plasma sintering often needs temperature and pressure with better adaptability to the material. Yao Jinyuan et al (publication No. CN1896303A) propose a strengthening method for preparing a diamond film on the surface of a tantalum spinneret by chemical vapor deposition, which effectively improves the hardness and the alkali corrosion resistance of the surface of the tantalum spinneret, but the method needs strict requirements on pressure, carbon source concentration and temperature. In conclusion, the direct or indirect application of diamond to material strengthening has clear feasibility.
Because the activation energy required for the conversion of graphite to diamond is high and the thermal stability of diamond at high temperatures is poor due to the special carbon structural properties of diamond, the efficient synthesis of diamond material directly from graphite is a great challenge. With the development of scientific technology, scholars in the related field have gradually accumulated a series of diamond preparation methods, which can be generally divided into two main categories: one is to convert non-diamond carbon in a diamond stable region into diamond, and the preparation of the diamond usually needs high temperature and high pressure conditions, for example, the Nayadong et al (publication No. CN103409746A) provides a method for cladding a nano-diamond composite coating by using a millisecond laser, which mixes microcrystalline graphite powder and catalyst powder in proportion and adopts laser irradiation with high energy density to obtain a high self-lubricating wear-resistant coating with high bonding strength and fine tissue; the other is that activated carbon groups in a diamond metastable zone are re-aggregated to form diamond, the preparation method of the diamond can be realized under the condition of low pressure, for example, Jinzengsun et al (publication number: CN1091996A) provides a method for preparing diamond seed crystals by using surface modified graphite as a raw material under the high-pressure environment by adopting a chemical vapor deposition method, and the large-particle high-pressure diamond with controllable growth quantity and size is obtained, compared with the traditional diamond synthesis pressure, the method can reduce the synthesis pressure of the diamond by 0.5GPa, and improve the conversion efficiency and the coarse particle size of the diamond. In summary, the synthesis of diamond from graphite at the present stage often requires extreme operating environments, such as high temperatures greater than 2000K and high pressures greater than 10GPa, and the above-mentioned methods for producing diamond often correspond to high costs and low yields due to these extreme operating environments. Therefore, how to efficiently synthesize nano-diamond through graphite has become one of the major technical bottlenecks that restrict further application of diamond in the field of surface strengthening at the present stage.
Disclosure of Invention
The invention aims to provide a composite strengthening method for synthesizing nano-diamond by laser induction, which can realize direct or indirect strengthening of the surface of a component and improve the comprehensive mechanical property of the surface of a vulnerable component while synthesizing the diamond by laser induction.
The invention aims to provide a composite strengthening method for synthesizing nano-diamond by laser induction, which is characterized by comprising the following steps: comprises the following steps:
(1) uniformly coating a carbon source on the surface of the component, and transmitting a laser beam by means of a carbon dioxide laser and continuously irradiating the surface of the carbon source to convert the carbon source into a graphene or activated carbon layer;
(2) laying a constraint layer above the carbon layer;
(3) a femtosecond laser is adopted to emit pulse laser beams, a heating laser is adopted to emit continuous laser beams, and the centers of two laser spots are ensured to be superposed and irradiated on the surface of the carbon layer;
(4) and carrying out laser shock composite strengthening operation on the three-dimensional numerical control mobile platform or the laser to the next strengthening position.
Preferably, in the step (1), a layer of carbon source is uniformly coated on the surface of the member to be reinforced, and the uniform coating mode includes a brush coating method, a spray coating method, a dip coating method, a blade coating method, a roll coating method, an injection method and a hot melting method, so as to realize efficient and uniform coating of the carbon source on the surface of the vulnerable member; before the carbon dioxide laser is irradiated, a heating platform is adopted to heat and solidify the carbon source, the heating temperature is not higher than 200 ℃, and the heating time is not more than 15 min.
Further, in the step (2), a constraint layer is laid on the graphene, and the constraint layer comprises BK-7 glass or quartz glass.
Further, in the step (3), a heating laser is used to emit a continuous laser beam, and the heating laser is a heating laser with a wavelength higher than 400nm and is used to provide an auxiliary heat source.
Furthermore, in the step (3), the process parameters of the femtosecond pulse laser include voltage, current, laser frequency, laser energy, laser wavelength, laser pulse width and spot size; the technological parameters of the semiconductor laser include the laser action distance and the laser spot size.
Preferred embodiments are as follows: in the step (1), the thickness range of the carbon layer is 1-10 mm; in the step (3), the wavelength of the femtosecond pulse laser is 248nm, the pulse width is 25ns, and the pulse energy is 300 mJ/Hz; the technological parameters of the semiconductor laser include the laser action distance and the laser spot size.
The strengthening mechanism of the invention is as follows:
the femtosecond pulse laser is a frequency-adjustable discontinuous laser beam generated by a femtosecond pulse laser, and the laser beam is irradiated on the surface of a material and interacts with the material, so that the surface of the material is ionized and generates plasma explosion, and then laser impact pressure of several GPa is generated, and nano diamond particles are generated. The heating laser can realize local accurate heating of the surface of the component, reduce harmful residual stress of the component and effectively increase the quantity of laser-induced synthesized nano-diamonds. The pulsed laser generated by the femtosecond laser and the laser generated by the heating laser act on CO at the same time2On the carbon layer prepared by the laser, on one hand, nano diamond particles are induced to generate, so that the direct strengthening of high-hardness diamond attached to the outer surface of a damageable component is realized, on the other hand, the surface of the carbon layer is ablated and generates plasma, and the plasma is generated on the transparent constraint layerUnder the action of the nano-diamond particles, the diffusion of the plasma is blocked, high-strength stress shock waves are generated, after the shock waves act on the diamond particles, the nano-diamond particles have a strengthening effect on the base material, so that crystal grains on the surface of the base material are refined, a compressive stress layer is formed on the surface of the base material, the gradient distribution of the size of the crystal grains in a strengthening area from the outside to the inside is realized, and the strength of the material can be effectively improved while the ductility of the material is not sacrificed.
The invention has the following advantages and beneficial effects:
(1) the femtosecond pulse laser can generate pulse laser which can induce the carbon layer to generate nano diamond particles;
(2) the shock wave pressure generated by the pulse laser acts on the surfaces of the diamond particles, so that the diamond is firmly and mechanically occluded with the surface and the subsurface of the component to be strengthened, and the surface hardness and the tribological performance of the component can be effectively improved;
(3) the heating laser can realize local accurate heating of the surface of the component, reduce harmful residual stress of the component and effectively improve the yield of laser-induced synthesized nano-diamond;
(4) by adopting the composite strengthening method for synthesizing the nano-diamond by laser induction, nano-diamond particles can be generated on the outer surface of the damageable component, and a microstructure with the grain size distributed in a gradient manner is generated on the surface layer of the component through the nano-diamond particles, so that the strength of the surface of the material is effectively improved while the ductility of the material is not sacrificed.
Drawings
Fig. 1 is a schematic diagram of a method for laser-producing a carbon layer according to the present invention.
Fig. 2 is a schematic diagram of the composite strengthening method for laser-induced synthesis of nano-diamond according to the present invention.
FIG. 3 is a schematic diagram of the strengthening effect of the diamond gradient microstructure according to the present invention.
In the figure: a member to be reinforced 1; a carbon source 2; a heating stage 3; a carbon dioxide laser 4; a carbon layer 5; sealing the chamber 6; a transparent constraining layer 7; a vacuum pump 8; a three-dimensional numerical control mobile platform 9; a femtosecond pulse laser 10; a semiconductor laser 11; the nano-diamond particles 12; the reinforced region 13.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
Example 1
Fig. 1 is a schematic diagram of a laser-based method for producing a carbon layer. A layer of polyimide 2 is uniformly coated on the surface of a 0.2mm pure copper plate 1 by adopting a glass rod rolling coating method, and the polyimide is placed on a heating platform 3 and is cured for 7 minutes at the temperature of 110 ℃. And (3) selecting 11% of light output power of a carbon dioxide laser 4, and continuously irradiating the laser beam on the surface of the cured polyimide to generate the graphene 5. Fig. 2 is a schematic diagram of a method for composite strengthening based on laser-induced synthesis of nanodiamonds. Placing a member to be strengthened with graphene 5 generated on the surface in a sealed chamber 6, placing a BK-7 glass restraint layer 7 above the graphene 5, starting a vacuum pump 8, carrying out vacuum pumping treatment on the sealed chamber 6, and placing the sealed chamber 6 on a three-dimensional numerical control mobile platform 9 when the interior of the sealed chamber is in a negative pressure state; by building a light path, the laser beam emitted by the femtosecond pulse laser 10 and the laser beam emitted by the semiconductor laser 11 can effectively irradiate the graphene 5, the centers of the laser spots of the laser beams of the femtosecond pulse laser 10 and the semiconductor laser 11 coincide, and 50% of the overlap ratio of the laser spots of the pulse laser is selected for strengthening operation; and after the laser impact is finished, opening the air valve, balancing the sealed cavity and the external air pressure, and taking out the pure copper plate 1.
Fig. 3 is a schematic diagram showing the strengthening effect of the diamond gradient microstructure. The strengthening mechanism of the pure copper plate is as follows: the pulse laser generated by the femtosecond pulse laser 10 and the laser generated by the heating laser 11 act on the surface of the graphene 5 prepared by the carbon dioxide laser 4 simultaneously, on one hand, nano diamond particles 12 are generated by induction, so that the direct strengthening of high-hardness diamond attached to the outer surface of the pure copper plate 1 is realized, on the other hand, the surface of the graphene 5 is ablated and generates plasma, the plasma is prevented from being diffused and generates high-strength stress shock waves under the action of the transparent constraint layer 7, after the shock waves act on the diamond particles 12, the nano diamond particles 12 have a strengthening effect on the pure copper plate 1, so that the surface grains of the pure copper plate 1 are refined, and a compression stress layer is formed on the surface of the pure copper plate, so that the gradient distribution of the strengthening region 13 from the surface to the inside is realized, and meanwhile, the gap structure of the nano diamond particles 12 can generate the gradient micro-structure distribution on the surface layer of the, the strength of the material is effectively improved while the ductility of the copper material is not sacrificed.
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 (8)
1. A composite strengthening method for synthesizing nano-diamond by laser induction is characterized in that: comprises the following steps:
(1) uniformly coating a carbon source on the surface of the component, and transmitting a laser beam by means of a carbon dioxide laser and continuously irradiating the surface of the carbon source to convert the carbon source into a graphene or activated carbon layer;
(2) laying a constraint layer above the carbon layer;
(3) a femtosecond laser is adopted to emit pulse laser beams, a heating laser is adopted to emit continuous laser beams, and the centers of two laser spots are ensured to be superposed and irradiated on the surface of the carbon layer;
(4) and carrying out laser shock composite strengthening operation on the three-dimensional numerical control mobile platform or the laser to the next strengthening position.
2. The composite strengthening method of laser-induced synthesis of nanodiamonds according to claim 1, wherein: in the step (1), a layer of carbon source is uniformly coated on the surface of the member to be reinforced, wherein the uniform coating mode comprises a brushing method, a spraying method, a dip coating method, a blade coating method, a rolling coating method, an injection method and a hot melting method, and the purpose is to realize efficient and uniform coating of the carbon source on the surface of the damageable member; before the carbon dioxide laser is irradiated, a heating platform is adopted to heat and solidify the carbon source, the heating temperature is not higher than 200 ℃, and the heating time is not more than 15 min.
3. The composite strengthening method of laser-induced synthesis of nanodiamonds according to claim 1 or 2, wherein: in the step (2), a restraint layer is laid on the graphene, and the restraint layer comprises BK-7 glass or quartz glass.
4. The composite strengthening method of laser-induced synthesis of nanodiamonds according to claim 1 or 2, wherein: in the step (2), a restraint layer is laid on the graphene, and the restraint layer comprises BK-7 glass or quartz glass.
5. The composite strengthening method of laser-induced synthesis of nanodiamonds according to claim 3, wherein: in the step (2), a restraint layer is laid on the graphene, and the restraint layer comprises BK-7 glass or quartz glass.
6. The composite strengthening method of laser induced synthesis of nanodiamonds according to claim 1, 2 or 5, wherein: in the step (3), a heating laser is adopted to emit continuous laser beams, wherein the heating laser is a heating laser with the wavelength higher than 400nm and is used for providing an auxiliary heat source.
7. The composite strengthening method of laser induced synthesis of nanodiamonds according to claim 1, 2 or 5, wherein: in the step (3), the process parameters of the femtosecond pulse laser include voltage, current, laser frequency, laser energy, laser wavelength, laser pulse width and spot size; the technological parameters of the semiconductor laser include the laser action distance and the laser spot size.
8. The composite strengthening method of laser-induced synthesis of nanodiamonds according to claim 6, wherein: in the step (3), the process parameters of the femtosecond pulse laser include voltage, current, laser frequency, laser energy, laser wavelength, laser pulse width and light spot size; the technological parameters of the semiconductor laser include the laser action distance and the laser spot size.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112647063A (en) * | 2020-11-30 | 2021-04-13 | 天津职业技术师范大学(中国职业培训指导教师进修中心) | DLC-nano diamond composite coating preparation method based on laser irradiation |
| CN114603762A (en) * | 2022-03-29 | 2022-06-10 | 北京理工大学 | Optical lens molding device and molding method |
| CN115703165A (en) * | 2021-08-09 | 2023-02-17 | 西湖大学 | A Method for Fabricating Ordered Subwavelength Nanostripes Using Femtosecond Laser |
| CN119274878A (en) * | 2024-11-04 | 2025-01-07 | 广东工业大学 | Improved laser-induced graphene and preparation method thereof |
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| CN112647063A (en) * | 2020-11-30 | 2021-04-13 | 天津职业技术师范大学(中国职业培训指导教师进修中心) | DLC-nano diamond composite coating preparation method based on laser irradiation |
| CN115703165A (en) * | 2021-08-09 | 2023-02-17 | 西湖大学 | A Method for Fabricating Ordered Subwavelength Nanostripes Using Femtosecond Laser |
| CN114603762A (en) * | 2022-03-29 | 2022-06-10 | 北京理工大学 | Optical lens molding device and molding method |
| CN119274878A (en) * | 2024-11-04 | 2025-01-07 | 广东工业大学 | Improved laser-induced graphene and preparation method thereof |
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