CN104498893B - Rapid preparation method of highly textured pyrolytic carbon film - Google Patents
Rapid preparation method of highly textured pyrolytic carbon film Download PDFInfo
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- CN104498893B CN104498893B CN201410800367.1A CN201410800367A CN104498893B CN 104498893 B CN104498893 B CN 104498893B CN 201410800367 A CN201410800367 A CN 201410800367A CN 104498893 B CN104498893 B CN 104498893B
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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
- C23C16/22—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
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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
- C23C16/44—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 method of coating
- C23C16/48—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 method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation
- C23C16/483—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 method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation using coherent light, UV to IR, e.g. lasers
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Abstract
The invention discloses a rapid preparation method of a highly textured pyrolytic carbon film. The method comprises the following steps: (1) flatting the surface of a carbon/carbon composite material target having the density of 1.85-1.90g/cm＜3＞, and clearing away oil stain on the surface of the target for later use; (2) putting the carbon/carbon composite material target on a flat graphite plate, enabling a laser beam to focus on the surface of the carbon/carbon composite material target, and keeping the laser beam perpendicular to the surface of the carbon/carbon composite material target; and (3) adopting high-power laser to quickly heat and gasify the carbon element in the carbon/carbon composite material target to form gaseous carbon atoms, and immobilizing the gaseous carbon atoms on a hot wall at a temperature greater than or equal to 2000 DEG C for growing, thereby obtaining the highly textured pyrolytic carbon film. According to the rapid preparation method, the high-power laser is adopted to promote the growth of the highly textured pyrolytic carbon film; the growth rate of the pyrolytic carbon film is increased to the range of 25-30 microns per second, and increased by 3 orders of magnitudes in contrast with 2*10＜-2＞ microns per second of a fluidized bed process.
Description
Technical field
The present invention relates to the preparation method of a kind of pyrolytic carbon thin film, a kind of highly-textured pyrolysis
The laser of C film promotes quick method of vapor-phase growing.
Background technology
Pyrolytic carbon has the physics of uniqueness, chemical property, such as low-density, neutron high temperature resistant, anti-
Radiation, good heat conductivity etc., be widely used in the fields such as space flight and aviation, nuclear energy, biomedicine.
Pyrolytic carbon typically uses organic gas to be at high temperature cracked to form, and available organic gas includes second
Alkynes, propylene, butadiene, methane etc., preparation method mainly has fixed bed and fluidised bed processes,
By controlling the process conditions such as carbon-source gas concentration, flow, pyrolysis temperature and fluidized state,
Obtain the pyrolytic carbon product of different structure.Due to carbon containing organic gas cracking reaction at high temperature
Belonging to complicated polymerization and fission reaction, the process of reaction cannot monitor in real time, cause pyrolytic carbon
There is the faults of construction such as carbon black in product, RESEARCH OF PYROCARBON TEXTURES is difficult to control to, and owing to being had by carbon containing
Diffusion and the transmission of machine gas control, and the growth rate of pyrolytic carbon is slow, typically exists
2×10-2μm/about s, it is difficult to meet the requirement quickly preparing high performance highly-textured pyrolytic carbon,
Need the pyrolytic carbon technology of preparing of Development of Novel.
With carbon/carbon compound material as raw material, by LASER HEATING, quickly prepare highly-textured
The method of pyrolytic carbon thin film, have not been reported in the prior art.
Summary of the invention
It is an object of the invention to overcome the deficiency of prior art to provide one quickly to prepare height
The method of texture pyrolytic carbon thin film.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, with carbon/carbon composite wood
Material base body is raw material, with high power laser as thermal source, is combined in carbon/carbon by laser beam focus
Body of material surface is heated, and after ablated surface forms opening, regulates laser focal, makes
Laser beam extends in carbon/carbon compound material base substrate, forms inverted cone-shaped cavity volume, in inverted cone
In shape cavity volume forming process, the carbon in carbon/carbon compound material base substrate is gasified by LASER HEATING, gas
Carbon after change is deposited on the wall of inverted cone-shaped cavity volume, is grown to serve as highly-textured pyrolytic carbon thin
Film.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, described carbon/carbon is combined
Body of material is to be dried and surfacing, the carbon/carbon compound material base substrate of cleaning.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, described carbon/carbon is combined
The density of body of material is 1.85～1.90g/cm3。
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, described high power laser
Device optical maser wavelength is 10.6 μm, and work output is 3～4.5kW.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, described high power laser
Device is needle plate discharge-type crossing current CO2Laser instrument.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, laser beam and carbon/
The position that carbon composite billet surface intersects, sprays noble gas.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, the noble gas sprayed
Pressure is 0.2-0.4MPa.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, described inverted cone-shaped holds
Chamber and opening constitute inverted cone-shaped hole, and the bottom surface in inverted cone-shaped hole is opening, its a diameter of 5～
10mm, the hole a height of 10～15mm in inverted cone-shaped hole.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, it is deposited on inverted cone
The thickness of the highly-textured pyrolytic carbon thin film on the wall of shape cavity volume is 50-150 μm, is preferably
100～120 μm.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, is deposited on inverted cone-shaped
Highly-textured pyrolytic carbon thin film on the wall of cavity volume is formed with carbon/carbon compound material base substrate and is tightly combined
Metallurgical binding.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, by spraying pressure be
The argon of 0.2-0.4MPa, protection workpiece is from oxidation.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, described inverted cone-shaped hole
Using laser drill mode molding, first laser beam focuses on the upper of carbon/carbon compound material base substrate
Below surface at 2mm, after burning opening, the focus of laser beam extends to upper surface vertically downward
At following 6mm, form inverted cone-shaped cavity volume, meanwhile, in carbon/carbon compound material base substrate
Carbon gasified by LASER HEATING, the carbon after gasification be deposited on inverted cone-shaped chamber wall temperature >=
The position of 2000 DEG C, is grown to serve as highly-textured pyrolytic carbon thin film.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, the carbon after gasification
Being deposited on temperature in inverted cone-shaped chamber wall is the position of 1800-2000 DEG C, is grown to serve as height and knits
Structure pyrolytic carbon thin film.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, described carbon/carbon is combined
Carbon in body of material is gasified by LASER HEATING and is grown to pyrolytic carbon thin film, and overall process is time-consumingly
2～5 seconds.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, described pyrolytic carbon thin film
Growth rate be 25～30 μm/s.
The fast preparation method of a kind of highly-textured pyrolytic carbon thin film of the present invention, is deposited on inverted cone-shaped
Highly-textured pyrolytic carbon thin film on the wall of cavity volume is after high-temperature process, and its degree of graphitization is >=85%,
The temperature of described high-temperature process is 2200-2250 DEG C.
The mechanism of the present invention is summarized as follows:
The present invention uses high power laser to act on carbon/carbon compound material target, on the one hand utilizes
Laser, at the high-energy gathered in short-term, makes the carbon of carbon/carbon compound material target regional area
Gasification, it is provided that the gaseous carbon atom needed for the growth of pyrolytic carbon thin film.On the other hand, heating rounding
The inner wall temperature of tapered hole is to >=2000 DEG C, it is provided that high temperature vapor phase growth bed, promotes that gaseous carbon is former
Sub-implantation, fast-growth are highly-textured pyrolytic carbon thin film.
Due to the fact that the above-mentioned process of employing, thus, have the advantage that and good effect:
1, the pure carbon-source gas that carbon/carbon compound material provides is used as target, compared to existing
Method is had to use the carbon-source gas that carbon containing organic gas cracking reaction at high temperature obtains, pure
Du Genggao, pyrolytic carbon product impurity content is less, and pyrolytic carbon membrane structure is more controlled.
2, the inverted cone-shaped hole opening used is big, cavity volume is little, makes in cavity volume by LASER HEATING gas
Gas after change is compressed under the high pressure of sprayed argon, forms malleation, promotes pyrolytic carbon
The fast deposition of thin film.
3, by spraying the argon that pressure is 0.2-0.4MPa, make workpiece by the height of LASER HEATING
Temperature position completely cuts off with surrounding air, and protection workpiece is from oxidation.Block inverted cone-shaped hole simultaneously
Opening so that in inverted cone-shaped hole, the vaporized carbon of generation is along inverted cone-shaped hole wall adsorption in turn, and
Rapidly deposition densification thus quickly to rise highly-textured pyrolytic carbon on the wall in inverted cone-shaped hole thin
Film.
4, high power laser is used, quickly heating, vaporized carbon atom make it be grown to height to knit
Structure pyrolytic carbon thin film, overall process is time-consumingly only 2～5 seconds, and the growth rate of pyrolytic carbon thin film reaches
To 25～30 μm/s, growth rate ratio the 2 × 10 of fluidised bed processes-2μm/s improves 3 numbers
Magnitude.
3, using high power laser, while Quick-gasifying carbon atom, heat growth bed, makes
Carbon atom after gasification is implantation, growth on the hot wall of temperature >=2000 DEG C, is conducive to obtaining height and knits
The pyrolytic carbon thin film of structure.
4, use the present invention, be 1.86g/cm by density3Carbon/carbon compound material target, warp
Wavelength be 10.6 μm, output be that the laser of 5.5kW promotes quickly to prepare highly-textured pyrolysis
C film, the growth rate of pyrolytic carbon thin film reaches 26 μm/s, than fluidised bed processes
2×10-2μm/s improves 3 orders of magnitude.
In sum, the fast preparation method of the highly-textured pyrolytic carbon thin film that the present invention provides, logical
Crossing employing high power laser, heat growth bed while Quick-gasifying carbon atom, after making gasification
Carbon atom implantation, growth on the hot wall of temperature >=2000 DEG C, it is thus achieved that highly-textured pyrolytic carbon is thin
Film.
Accompanying drawing explanation
Accompanying drawing 1 is the quick vapor phase growth principle signal of the highly-textured pyrolytic carbon thin film of the present invention
Figure
The accompanying drawing 2 highly-textured pyrolytic carbon thin film prepared by embodiment 3
In Fig. 1: 1-carbon/carbon compound material, 2-laser beam, 3-highly-textured pyrolytic carbon thin film.
In Fig. 2: 1-carbon/carbon compound material, 3-highly-textured pyrolytic carbon thin film.
Detailed description of the invention
In embodiment, the sedimentation rate of pyrolytic carbon is the thickness by measuring carbon fiber surface pyrolytic carbon
Degree, then obtain divided by sedimentation time.
Embodiment 1:
(1) it is 1.85g/cm by density3Carbon/carbon compound material target material surface processing smooth,
Clean surface oil stain standby；
(2) by graphite cake whole for carbon/carbon compound material target horizontalization, make laser beam focus in
Carbon/carbon compound material target material surface, laser beam and carbon/carbon compound material target material surface keep hanging down
Directly；
(3) laser beam focus is heated in carbon/carbon compound material billet surface, exist simultaneously
The position that laser beam intersects with carbon/carbon compound material billet surface, spouting pressure is 0.2MPa's
Noble gas；After ablated surface forms opening, continue to spray noble gas, and regulate laser
Focal length makes laser beam extend in carbon/carbon compound material base substrate, forms inverted cone-shaped cavity volume, institute
Stating inverted cone-shaped cavity volume and constitute inverted cone-shaped hole with opening, the bottom surface in inverted cone-shaped hole is out
Mouthful, its a diameter of 7mm, a height of 13mm in hole in inverted cone-shaped hole.Inverted cone-shaped hole opening is big,
Cavity volume is little, makes the gas after being gasified by LASER HEATING in cavity volume be subject under the high pressure spraying argon
To compression, form malleation, promote the fast deposition of pyrolytic carbon thin film；
(4) high power laser is used, in quickly heating, gasification carbon/carbon compound material target
Carbon, forms gaseous carbon atom, and is implantation on >=2000 DEG C of hot walls in temperature, grows into
For highly-textured pyrolytic carbon thin film.Control optical maser wavelength be 10.6 μm, output be 5.2kW,
Heat time heating time is 3 seconds, and the thickness obtaining pyrolytic carbon thin film is 75 μm.
The present invention promotes the vapor phase growth of highly-textured pyrolytic carbon thin film by using high power laser
Process, makes the growth rate of pyrolytic carbon thin film reach 25 μm/s, and pyrolytic carbon thin film is through 2200 DEG C
Degree of graphitization after high-temperature process is 86.3%, and growth rate is than fluidised bed processes
2×10-2μm/s improves 3 orders of magnitude.
Embodiment 2:
(1) it is 1.88g/cm by density3Carbon/carbon compound material target material surface processing smooth,
Clean surface oil stain standby；
(2) by graphite cake whole for carbon/carbon compound material target horizontalization, make laser beam focus in
Carbon/carbon compound material target material surface, laser beam and carbon/carbon compound material target material surface keep hanging down
Directly；
(3) laser beam focus is heated in carbon/carbon compound material billet surface, exist simultaneously
The position that laser beam intersects with carbon/carbon compound material billet surface, spouting pressure is 0.3MPa's
Noble gas；After ablated surface forms opening, continue to spray noble gas, and regulate laser
Focal length makes laser beam extend in carbon/carbon compound material base substrate, forms inverted cone-shaped cavity volume, institute
Stating inverted cone-shaped cavity volume and constitute inverted cone-shaped hole with opening, the bottom surface in inverted cone-shaped hole is out
Mouthful, its a diameter of 6mm, a height of 10mm in hole in inverted cone-shaped hole.Inverted cone-shaped hole opening is big,
Cavity volume is little, makes the gas after being gasified by LASER HEATING in cavity volume be subject under the high pressure spraying argon
To compression, form malleation, promote the fast deposition of pyrolytic carbon thin film；
(4) high power laser is used, in quickly heating, gasification carbon/carbon compound material target
Carbon, formed gaseous carbon atom, and on the hot wall of temperature >=2000 DEG C implantation, be grown to serve as
Highly-textured pyrolytic carbon thin film.Control optical maser wavelength be 10.6 μm, output be 4.6kW,
Heat time heating time is 2 seconds, and the thickness obtaining pyrolytic carbon thin film is 50 μm.
The present invention promotes the vapor phase growth of highly-textured pyrolytic carbon thin film by using high power laser
Process, makes the growth rate of pyrolytic carbon thin film reach 25 μm/s, and pyrolytic carbon thin film is through 2200 DEG C
Degree of graphitization after high-temperature process is 87.1%, and growth rate is than fluidised bed processes
2×10-2μm/s improves 3 orders of magnitude.
Embodiment 3:
(1) it is 1.86g/cm by density3Carbon/carbon compound material target material surface processing smooth,
Clean surface oil stain standby；
(2) by graphite cake whole for carbon/carbon compound material target horizontalization, make laser beam focus in
Carbon/carbon compound material target material surface, laser beam and carbon/carbon compound material target material surface keep hanging down
Directly；
(3) laser beam focus is heated in carbon/carbon compound material billet surface, exist simultaneously
The position that laser beam intersects with carbon/carbon compound material billet surface, spouting pressure is 0.4MPa's
Noble gas；After ablated surface forms opening, continue to spray noble gas, and regulate laser
Focal length makes laser beam extend in carbon/carbon compound material base substrate, forms inverted cone-shaped cavity volume, institute
Stating inverted cone-shaped cavity volume and constitute inverted cone-shaped hole with opening, the bottom surface in inverted cone-shaped hole is out
Mouthful, its a diameter of 9mm, a height of 15mm in hole in inverted cone-shaped hole.Inverted cone-shaped hole opening is big,
Cavity volume is little, makes the gas after being gasified by LASER HEATING in cavity volume be subject under the high pressure spraying argon
To compression, form malleation, promote the fast deposition of pyrolytic carbon thin film；
(4) high power laser is used, in quickly heating, gasification carbon/carbon compound material target
Carbon, formed gaseous carbon atom, and on the hot wall of temperature >=2000 DEG C implantation, be grown to serve as
Highly-textured pyrolytic carbon thin film.Control optical maser wavelength be 10.6 μm, output be 5.5kW,
Heat time heating time is 4 seconds, and the thickness obtaining pyrolytic carbon thin film is 104 μm.
The present invention promotes the vapor phase growth of highly-textured pyrolytic carbon thin film by using high power laser
Process, makes the growth rate of pyrolytic carbon thin film reach 26 μm/s, and pyrolytic carbon thin film is through 2200 DEG C
Degree of graphitization after high-temperature process is 85.2%, and growth rate is than fluidised bed processes
2×10-2μm/s improves 3 orders of magnitude.
Embodiment 4:
(1) it is 1.89g/cm by density3Carbon/carbon compound material target material surface processing smooth,
Clean surface oil stain standby；
(2) by graphite cake whole for carbon/carbon compound material target horizontalization, make laser beam focus in
Carbon/carbon compound material target material surface, laser beam and carbon/carbon compound material target material surface keep hanging down
Directly；
(3) laser beam focus is heated in carbon/carbon compound material billet surface, exist simultaneously
The position that laser beam intersects with carbon/carbon compound material billet surface, spouting pressure is 0.25MPa
Noble gas；After ablated surface forms opening, continue to spray noble gas, and regulate sharp
Light focal length makes laser beam extend in carbon/carbon compound material base substrate, forms inverted cone-shaped cavity volume,
Described inverted cone-shaped cavity volume constitutes inverted cone-shaped hole with opening, and the bottom surface in inverted cone-shaped hole is out
Mouthful, its a diameter of 9mm, a height of 14mm in hole in inverted cone-shaped hole.Inverted cone-shaped hole opening is big,
Cavity volume is little, makes the gas after being gasified by LASER HEATING in cavity volume be subject under the high pressure spraying argon
To compression, form malleation, promote the fast deposition of pyrolytic carbon thin film；
(4) high power laser is used, in quickly heating, gasification carbon/carbon compound material target
Carbon, formed gaseous carbon atom, and on the hot wall of temperature >=2000 DEG C implantation, be grown to serve as
Highly-textured pyrolytic carbon thin film.Control optical maser wavelength be 10.6 μm, output be 5.3kW,
Heat time heating time is 4 seconds, and the thickness obtaining pyrolytic carbon thin film is 116 μm.
The present invention promotes the vapor phase growth of highly-textured pyrolytic carbon thin film by using high power laser
Process, makes the growth rate of pyrolytic carbon thin film reach 29 μm/s, and pyrolytic carbon thin film is through 2200 DEG C
Degree of graphitization after high-temperature process is 86.7%, and growth rate is than fluidised bed processes
2×10-2μm/s improves 3 orders of magnitude.
Embodiment 5:
(1) it is 1.90g/cm by density3Carbon/carbon compound material target material surface processing smooth,
Clean surface oil stain standby；
(2) by graphite cake whole for carbon/carbon compound material target horizontalization, make laser beam focus in
Carbon/carbon compound material target material surface, laser beam and carbon/carbon compound material target material surface keep hanging down
Directly；
(3) laser beam focus is heated in carbon/carbon compound material billet surface, exist simultaneously
The position that laser beam intersects with carbon/carbon compound material billet surface, spouting pressure is 0.35MPa
Noble gas；After ablated surface forms opening, continue to spray noble gas, and regulate sharp
Light focal length makes laser beam extend in carbon/carbon compound material base substrate, forms inverted cone-shaped cavity volume,
Described inverted cone-shaped cavity volume constitutes inverted cone-shaped hole with opening, and the bottom surface in inverted cone-shaped hole is out
Mouthful, its a diameter of 5mm, a height of 11mm in hole in inverted cone-shaped hole.Inverted cone-shaped hole opening is big,
Cavity volume is little, makes the gas after being gasified by LASER HEATING in cavity volume be subject under the high pressure spraying argon
To compression, form malleation, promote the fast deposition of pyrolytic carbon thin film；
(4) high power laser is used, in quickly heating, gasification carbon/carbon compound material target
Carbon, formed gaseous carbon atom, and on the hot wall of temperature >=2000 DEG C implantation, be grown to serve as
Highly-textured pyrolytic carbon thin film.Control optical maser wavelength be 10.6 μm, output be 5.1kW,
Heat time heating time is 2 seconds, and the thickness obtaining pyrolytic carbon thin film is 60 μm.
The present invention promotes the vapor phase growth of highly-textured pyrolytic carbon thin film by using high power laser
Process, makes the growth rate of pyrolytic carbon thin film reach 30 μm/s, and pyrolytic carbon thin film is through 2200 DEG C
Degree of graphitization after high-temperature process is 85.1%, and growth rate is than fluidised bed processes
2×10-2μm/s improves 3 orders of magnitude.
Embodiment 6:
(1) it is 1.86g/cm by density3Carbon/carbon compound material target material surface processing smooth,
Clean surface oil stain standby；
(2) by graphite cake whole for carbon/carbon compound material target horizontalization, make laser beam focus in
Carbon/carbon compound material target material surface, laser beam and carbon/carbon compound material target material surface keep hanging down
Directly；
(3) laser beam focus is heated in carbon/carbon compound material billet surface, exist simultaneously
The position that laser beam intersects with carbon/carbon compound material billet surface, spouting pressure is 0.28MPa
Noble gas；After ablated surface forms opening, continue to spray noble gas, and regulate sharp
Light focal length makes laser beam extend in carbon/carbon compound material base substrate, forms inverted cone-shaped cavity volume,
Described inverted cone-shaped cavity volume constitutes inverted cone-shaped hole with opening, and the bottom surface in inverted cone-shaped hole is out
Mouthful, its a diameter of 8mm, a height of 14mm in hole in inverted cone-shaped hole.Inverted cone-shaped hole opening is big,
Cavity volume is little, makes the gas after being gasified by LASER HEATING in cavity volume be subject under the high pressure spraying argon
To compression, form malleation, promote the fast deposition of pyrolytic carbon thin film；
(4) high power laser is used, in quickly heating, gasification carbon/carbon compound material target
Carbon, formed gaseous carbon atom, and on the hot wall of temperature >=2000 DEG C implantation, be grown to serve as
Highly-textured pyrolytic carbon thin film.Control optical maser wavelength be 10.6 μm, output be 4.8kW,
Heat time heating time is 4 seconds, and the thickness obtaining pyrolytic carbon thin film is 101.2 μm.
The present invention promotes the vapor phase growth of highly-textured pyrolytic carbon thin film by using high power laser
Process, makes the growth rate of pyrolytic carbon thin film reach 25.3 μm/s, and pyrolytic carbon thin film is through 2200
Degree of graphitization after DEG C high-temperature process is 86.2%, and growth rate is than fluidised bed processes
2×10-2μm/s improves 3 orders of magnitude.
Embodiment 7:
(1) it is 1.87g/cm by density3Carbon/carbon compound material target material surface processing smooth,
Clean surface oil stain standby；
(2) by graphite cake whole for carbon/carbon compound material target horizontalization, make laser beam focus in
Carbon/carbon compound material target material surface, laser beam and carbon/carbon compound material target material surface keep hanging down
Directly；
(3) laser beam focus is heated in carbon/carbon compound material billet surface, exist simultaneously
The position that laser beam intersects with carbon/carbon compound material billet surface, spouting pressure is 0.36MPa
Noble gas；After ablated surface forms opening, continue to spray noble gas, and regulate sharp
Light focal length makes laser beam extend in carbon/carbon compound material base substrate, forms inverted cone-shaped cavity volume,
Described inverted cone-shaped cavity volume constitutes inverted cone-shaped hole with opening, and the bottom surface in inverted cone-shaped hole is out
Mouthful, its a diameter of 6mm, a height of 13mm in hole in inverted cone-shaped hole.Inverted cone-shaped hole opening is big,
Cavity volume is little, makes the gas after being gasified by LASER HEATING in cavity volume be subject under the high pressure spraying argon
To compression, form malleation, promote the fast deposition of pyrolytic carbon thin film；
(4) high power laser is used, in quickly heating, gasification carbon/carbon compound material target
Carbon, formed gaseous carbon atom, and on the hot wall of temperature >=2000 DEG C implantation, be grown to serve as
Highly-textured pyrolytic carbon thin film.Control optical maser wavelength be 10.6 μm, output be 4.6kW,
Heat time heating time is 3 seconds, and the thickness obtaining pyrolytic carbon thin film is 80 μm.
The present invention promotes the vapor phase growth of highly-textured pyrolytic carbon thin film by using high power laser
Process, makes the growth rate of pyrolytic carbon thin film reach 26.6 μm/s, and pyrolytic carbon thin film is through 2200
Degree of graphitization after DEG C high-temperature process is 86.9%, and growth rate is than fluidised bed processes
2×10-2μm/s improves 3 orders of magnitude.
Embodiment 8:
(1) it is 1.86g/cm by density3Carbon/carbon compound material target material surface processing smooth,
Clean surface oil stain standby；
(2) by graphite cake whole for carbon/carbon compound material target horizontalization, make laser beam focus in
Carbon/carbon compound material target material surface, laser beam and carbon/carbon compound material target material surface keep hanging down
Directly；
(3) laser beam focus is heated in carbon/carbon compound material billet surface, exist simultaneously
The position that laser beam intersects with carbon/carbon compound material billet surface, spouting pressure is 0.4MPa's
Noble gas；After ablated surface forms opening, continue to spray noble gas, and regulate laser
Focal length makes laser beam extend in carbon/carbon compound material base substrate, forms inverted cone-shaped cavity volume, institute
Stating inverted cone-shaped cavity volume and constitute inverted cone-shaped hole with opening, the bottom surface in inverted cone-shaped hole is out
Mouthful, its a diameter of 6mm, a height of 13mm in hole in inverted cone-shaped hole.Inverted cone-shaped hole opening is big,
Cavity volume is little, makes the gas after being gasified by LASER HEATING in cavity volume be subject under the high pressure spraying argon
To compression, form malleation, promote the fast deposition of pyrolytic carbon thin film；
(3) high power laser is used, in quickly heating, gasification carbon/carbon compound material target
Carbon, formed gaseous carbon atom, and on the hot wall of temperature >=2000 DEG C implantation, be grown to serve as
Highly-textured pyrolytic carbon thin film.Control optical maser wavelength be 10.6 μm, output be 4.7kW,
Heat time heating time is 3 seconds, and the thickness obtaining pyrolytic carbon thin film is 75.3 μm.
The present invention promotes the vapor phase growth of highly-textured pyrolytic carbon thin film by using high power laser
Process, makes the growth rate of pyrolytic carbon thin film reach 25.1 μm/s, and pyrolytic carbon thin film is through 2200
Degree of graphitization after DEG C high-temperature process is 85.4%, and growth rate is than fluidised bed processes
2×10-2μm/s improves 3 orders of magnitude.
Claims (10)
1. the fast preparation method of a highly-textured pyrolytic carbon thin film, it is characterised in that: with carbon/
Carbon composite base substrate is raw material, with high power laser as thermal source, by laser beam focus in carbon
/ carbon composite billet surface heats, in laser beam and carbon/carbon compound material billet surface
The position intersected, sprays noble gas；After ablated surface forms opening, regulate laser focal,
Make laser beam extend in carbon/carbon compound material base substrate, form inverted cone-shaped cavity volume, at rounding
In taper cavity volume forming process, the carbon in carbon/carbon compound material base substrate is gasified by LASER HEATING,
Carbon after gasification is deposited on the wall of inverted cone-shaped cavity volume, is grown to serve as highly-textured pyrolytic carbon
Thin film；The noble gas pressure sprayed is 0.2-0.4MPa.
The quickly side of preparation of a kind of highly-textured pyrolytic carbon thin film the most according to claim 1
Method, it is characterised in that: the density of described carbon/carbon compound material base substrate is 1.85～1.90g/cm3。
The quickly side of preparation of a kind of highly-textured pyrolytic carbon thin film the most according to claim 1
Method, it is characterised in that: described high power laser optical maser wavelength is 10.6 μm, work output
Power is 3～4.5kW.
The quickly side of preparation of a kind of highly-textured pyrolytic carbon thin film the most according to claim 3
Method, it is characterised in that: described high power laser is needle plate discharge-type crossing current CO2Laser instrument.
5. according to a kind of highly-textured pyrolytic carbon thin film described in claim 1-4 any one
Fast preparation method, it is characterised in that: described inverted cone-shaped cavity volume constitutes inverted cone-shaped with opening
Hole, the bottom surface in inverted cone-shaped hole is opening, its a diameter of 5～10mm, inverted cone-shaped hole
Hole a height of 10～15mm.
The quickly side of preparation of a kind of highly-textured pyrolytic carbon thin film the most according to claim 5
Method, it is characterised in that: described inverted cone-shaped hole uses laser drill mode molding, and laser beam is first
First focus at below the upper surface of carbon/carbon compound material base substrate 2mm, after burning opening, swash
The focus of light beam extends at below upper surface 6mm vertically downward, forms inverted cone-shaped cavity volume,
Meanwhile, the carbon in carbon/carbon compound material base substrate is gasified by LASER HEATING, the carbon after gasification
Element deposition is the position of temperature >=2000 DEG C in inverted cone-shaped chamber wall, is grown to serve as highly-textured
Pyrolytic carbon thin film.
The quickly side of preparation of a kind of highly-textured pyrolytic carbon thin film the most according to claim 5
Method, it is characterised in that: the highly-textured pyrolytic carbon thin film being deposited on the wall of inverted cone-shaped cavity volume
Thickness is 50～150 μm.
The quickly side of preparation of a kind of highly-textured pyrolytic carbon thin film the most according to claim 7
Method, it is characterised in that: the carbon in carbon/carbon compound material base substrate is gasified by LASER HEATING, gasification
After carbon be deposited on the wall of inverted cone-shaped cavity volume, be grown to serve as highly-textured pyrolytic carbon thin
Film, overall process is time-consumingly 2～5 seconds.
The quickly side of preparation of a kind of highly-textured pyrolytic carbon thin film the most according to claim 8
Method, it is characterised in that: the growth rate of described pyrolytic carbon thin film is 25～30 μm/s.
The quick preparation of a kind of highly-textured pyrolytic carbon thin film the most according to claim 6
Method, it is characterised in that: the highly-textured pyrolytic carbon thin film being deposited on the wall of inverted cone-shaped cavity volume
After high-temperature process, its degree of graphitization is >=85%, the temperature of described high-temperature process be 2200～
2250℃。
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Citations (3)
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|---|---|---|---|---|
| SU1427766A1 (en) * | 1986-12-30 | 1990-12-15 | Предприятие П/Я М-5409 | Method of producing highly oriented pyrrographite |
| WO1999035297A1 (en) * | 1998-01-02 | 1999-07-15 | Dana Corporation | Laser phase transformation and ion implantation in metals |
| CN102320853A (en) * | 2011-08-24 | 2012-01-18 | 中南大学 | Preparation method of carbon-based composite cathode material with highly-oriented emission characteristic |
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| KR101353126B1 (en) * | 2011-10-11 | 2014-02-17 | 성균관대학교산학협력단 | Solder resist composition, board for package comprising solder resist opening using the composition, and method for preparing the board for package |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1427766A1 (en) * | 1986-12-30 | 1990-12-15 | Предприятие П/Я М-5409 | Method of producing highly oriented pyrrographite |
| WO1999035297A1 (en) * | 1998-01-02 | 1999-07-15 | Dana Corporation | Laser phase transformation and ion implantation in metals |
| CN102320853A (en) * | 2011-08-24 | 2012-01-18 | 中南大学 | Preparation method of carbon-based composite cathode material with highly-oriented emission characteristic |
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