CN110557936B - Diamond microchannel Cu-based CVD diamond heat-sink sheet and preparation method thereof - Google Patents
Diamond microchannel Cu-based CVD diamond heat-sink sheet and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a diamond microchannel Cu-based CVD diamond heat-sinking sheet and a preparation method thereof, which sequentially comprise a Cu substrate, a micro through hole template and a CVD diamond film from bottom to top, wherein nano diamond particles are arranged between the Cu substrate and the micro through hole template, a diamond microchannel array is embedded in the Cu substrate, the diameter of each diamond microchannel is 0.3-0.5 mm, and the distance between the microchannels is 2-3 mm. The heat dissipation effect of the invention is superior to that of traditional heat sink sheets such as Ag, Cu, Al and the like; the heat dissipation performance of the micro-channel Cu-based diamond heat sink sheet is better; the nucleation density and the growth rate of the diamond in the micro through hole are greatly improved; the CVD selective growth of the diamond film is realized in the micro-through hole.
Description
Technical Field
The invention belongs to the technical field of diamond material application, and particularly relates to a diamond micro-channel Cu-based CVD diamond heat-sink sheet and a preparation method thereof.
Background
With the rapid progress of microelectronic integration technology and high-density packaging technology of hollow printed boards, the design and production of electronic components and electronic systems are continuously developing toward miniaturization, light weight, compactness and high efficiency. The power density of electronic components and electronic systems is becoming higher and higher, resulting in a large amount of heat generated during operation, which if not removed in time, will seriously affect the working stability and safety and reliability of electronic components and electronic systems, and thus the heat dissipation problem becomes a critical issue to be solved urgently in the electronic technology field. Ag. The traditional electronic packaging heat dissipation materials such as Cu, Al and the like have large thermal expansion coefficient, and the expansion is easy to cause circulating thermal stress to damage electronic components after being heated, so that the requirements of the current advanced electronic technology on the packaging heat dissipation materials can not be obviously met.
The thermal conductivity of the diamond can reach 2000W/(m.K) to the maximum, the diamond is compounded with metal Cu with high thermal conductivity, so that an ideal novel electronic packaging heat dissipation material with high thermal conductivity, low expansion and low density can be expected to be obtained, the thermal conductivity at room temperature is expected to reach 450W/(m.K) -1200W/(m.K), and the thermal expansion coefficient is 4 multiplied by 10-6～6×10-6K-1The Cu-based diamond heat sink sheet is matched with semiconductor materials such as Si, GaAs and the like, and can well solve the heat dissipation problem of modern high-power and high-density electronic components and electronic systems.
Disclosure of Invention
The invention aims to solve the technical problem of providing a diamond micro-channel Cu-based CVD diamond heat sink sheet and a preparation method thereof aiming at the defects in the prior art, and the heat dissipation problem of modern high-power and high-density electronic components and electronic systems is solved by utilizing the high thermal conductivity of diamond.
The invention adopts the following technical scheme:
the utility model provides a diamond microchannel Cu base CVD diamond heat sinks piece, is thin from supreme Cu base, little through-hole template and CVD diamond of including in proper order down, is provided with nanometer diamond granule between Cu base and the little through-hole template, inlays in the Cu base and has diamond microchannel array, and diamond microchannel's diameter is 0.3~0.5mm, and the microchannel interval is 2~3 mm.
Specifically, the diameter of the Cu substrate is 10-20 mm, and the thickness is 0.5-1 mm.
Specifically, the diamond micro-channel shape comprises a circle, a regular triangle, a square, a regular hexagon or a regular octagon.
Specifically, the nano-diamond particles are spherical structures, and the average particle size is 2-6 nm.
Specifically, the thickness of the CVD diamond film is 0.2-0.3 mm.
The invention also provides a preparation method of the diamond micro-channel Cu-based CVD diamond heat-sink sheet, which comprises the following steps:
s1, cutting an oxygen-free copper matrix with the purity of 99.99-99.999% and the diameter of 10-20 mm into a copper sheet with the diameter of 0.5-1 mm as a Cu substrate in a linear mode, and cleaning the surface of the Cu substrate;
s2, manufacturing a micro through hole template, wherein the micro through hole template is made of oxygen-free copper with the same specification as the Cu substrate;
s3, assembling nano diamond particles on the surface of the Cu substrate in an electrostatic manner, and improving the nucleation density of diamond on the gold Cu substrate, wherein the nano diamond particles are spherical and have the average particle size of 2-6 nm;
s4, stacking the micro-through-hole templates on a Cu substrate, and selectively growing a diamond film by adopting a template method CVD, wherein the thickness of the CVD diamond film is 0.2-0.3 mm;
s5, chemically and mechanically polishing the diamond surface to enable the diamond on the surface to be flat;
s6, peeling the Cu substrate, and slightly prying the Cu substrate along the gap between the Cu substrate and the micro through hole template by using a pair of tweezers to remove the Cu substrate; or soaking the sample in a ferric trichloride solution for 30-60 s to remove the Cu substrate.
Specifically, step S2 specifically includes:
s201, punching and punching a Cu substrate by adopting a mechanical punching and punching, hydraulic punching, laser punching or drilling process of a drilling machine, wherein the diameter of each micro through hole is 0.3-0.5 mm, and the channel spacing is 2-3 mm; the shape of the micro through hole comprises a circle, a regular triangle, a square, a regular hexagon or a regular octagon;
s202, slightly corroding the Cu substrate and the micro through hole template for 3-5 min by using a hydrochloric acid solution with the volume ratio of 0.5%, and removing processing burrs in an oxide film and the micro through holes;
s203, sequentially using acetone, alcohol and deionized water to ultrasonically clean the substrate and the micro through hole template for 3-5 min, removing organic matters on the surface of the Cu substrate, and drying;
s204, dispersing the nano-diamond powder subjected to surface modification by heat treatment in deionized water, performing ultrasonic treatment for 30-50 min to form a nano-diamond dispersion solution with the concentration of 3.0-7.1 g/ml, immersing a Cu substrate in the prepared nano-diamond dispersion solution, and performing ultrasonic oscillation for 10-15 min;
s205, taking out the Cu substrate, putting the Cu substrate into deionized water to wash away redundant nano diamond particles, and then drying the Cu substrate;
and S206, stacking the micro through hole template on the Cu substrate and fixing the micro through hole template by using a clamp.
Specifically, step S3 specifically includes:
s301, carbonizing filament in CH4、H2Keeping the temperature of 2500 ℃ or higher for a period of time in the atmosphere, wherein the total flow rate of the gas is 500-600 sccm and CH4The percentage of the carbonization reaction is 3-5%, the air pressure of a reaction chamber is 4.5-5.0 Kpa, and the carbonization reaction is carried out for 2-3 hours fully;
s302, installing a filament, wherein the filament is a spiral coil, the diameter of the filament is 0.4-0.6 mm, the inner diameter of the spiral is 1-1.5 mm, the number of turns is 12-15, and the distance between two adjacent turns is 0.5-1 mm;
s303, placing the micro through hole template on a molybdenum support in the reaction cavity;
s304, adjusting the position of the micro through hole template to align the micro through hole with the filament;
s305, vacuumizing;
s306, starting an infrared thermometer, and monitoring the temperature of the surface of the micro through hole template;
s307, with CH4、H2And as a reaction gas, selectively growing a diamond film on the micro-through hole template by CVD.
Further, in step S307, the temperature of the hot wire is 2200 + -100 ℃, the distance between the hot wire and the substrate is 10 + -1 mm, and the temperature of the substrate is 750 +/-50 ℃, deposition pressure of 2-3 Kpa, growth time of 2-3 h, CH4、H2The total flow rate is 500-600 sccm, CH4The percentage of (B) is 0.5% -3%.
Specifically, in step S4, the CVD diamond film growth method includes hot filament CVD, combustion flame CVD, electron-assisted CVD, microwave plasma CVD (mpcvd), radio frequency plasma CVD, direct current plasma CVD, or hybrid physical chemical vapor CVD.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the diamond microchannel Cu-based CVD diamond heat sink sheet, diamond with high thermal conductivity is used as a heat sink, and the heat dissipation effect is superior to that of traditional heat sink sheets such as Ag, Cu and Al; compared with the traditional Cu-based diamond film heat sink sheet with the serial structure of the upper layer and the lower layer, the diamond micro-channel Cu-based diamond heat sink sheet forms a longitudinal diamond heat dissipation channel on the Cu substrate, and as shown in figure 4, the problem of limitation of large heat of the Cu substrate on the heat dissipation performance of the heat sink sheet is solved; compared with a diamond powder particle/copper composite heat sink sheet, the micro-channel Cu-based diamond heat sink sheet forms a continuous diamond heat dissipation channel on a Cu substrate, so that the problem of limitation on heat dissipation performance of the heat sink sheet caused by continuous distribution of diamond powder particles in Cu is solved, and the heat dissipation performance of the micro-channel Cu-based diamond heat sink sheet is better; the nano diamond particles are assembled on the surface of the Cu substrate at the bottom of the micro through hole in an electrostatic manner, so that the nucleation density and the growth rate of diamond in the micro through hole are greatly improved; and the nucleation density and the growth rate of diamond on the surface of the micro-through hole template which is not processed are low, and the CVD selective growth of the diamond film is realized in the micro-through hole, as shown in figure 6.
Furthermore, the substrate of the heat sink sheet is a Cu substrate, the Cu has good heat conduction performance and low price, the diamond and the Cu are compounded, an ideal novel electronic packaging heat dissipation material with high heat conduction, low expansion and low density is expected to be obtained, the heat conduction coefficient is expected to reach 450W/(m.K) -1200W/(m.K) at room temperature, and the thermal expansion coefficient is 4 multiplied by 10-6～6×10-6K-1The material is matched with semiconductor materials such as Si, GaAs and the like, and is particularly suitable for manufacturing substrates and heat conduction materials of high-speed operation or high-power semiconductor chips.
Furthermore, the longitudinal diamond heat dissipation channel is formed on the Cu substrate by the diamond micro-channel Cu-based diamond heat sink sheet, and compared with the traditional Cu-based diamond film heat sink sheet with a serial structure of an upper layer and a lower layer, the limitation of large heat of the Cu substrate on the heat dissipation performance of the heat sink sheet is solved; compared with a diamond powder particle/copper composite heat sink sheet, the micro-channel Cu-based diamond heat sink sheet forms a continuous diamond heat dissipation channel on a Cu substrate, and the problem of limitation on heat dissipation performance of the heat sink sheet caused by continuous distribution of diamond powder particles in Cu is solved.
Furthermore, diamond nano particles are assembled on the surface of the Cu substrate at the bottom of the micro through hole in an electrostatic manner, so that the nucleation density and the growth rate of diamond in the micro through hole are greatly improved; and the nucleation density and the growth rate of diamond on the surface of the untreated micro-through hole template are low, and the CVD selective growth of the diamond film is realized in the micro-through hole.
Furthermore, the surface of the heat sink is a CVD diamond film, the thermal conductivity of the diamond can reach 2000W/(m.K) at most, and the CVD diamond film is continuously grown to form a continuous transverse diamond heat dissipation channel, so that the heat dissipation performance of the heat sink is further improved by transverse heat dissipation of the diamond film.
A method for preparing a diamond micro-channel Cu-based CVD diamond heat sink sheet is characterized in that a longitudinal diamond heat dissipation channel is formed on a Cu substrate, and compared with a traditional Cu-based diamond film heat sink sheet with an upper layer and a lower layer in a series structure, the problem that the heat dissipation performance of the heat sink sheet is limited by a large heat group of the Cu substrate is solved; in addition, diamond nano particles are assembled on the surface of the Cu substrate at the bottom of the micro through hole in an electrostatic manner, so that the nucleation density and the growth rate of diamond in the micro through hole are greatly improved; and the nucleation density and the growth rate of diamond on the surface of the untreated micro-through hole template are low, and the CVD selective growth of the diamond film is realized in the micro-through hole.
Further, punching and punching a Cu substrate by adopting a mechanical punching and punching, hydraulic punching, laser punching or drilling machine drilling process to form a micro through hole array template on the Cu substrate, wherein the diameter of each micro through hole is 0.3-0.5 mm, the channel spacing is 2-3 mm, and the shape of each micro through hole comprises a circle, a regular triangle, a square, a regular hexagon or a regular octagon; slightly corroding the Cu substrate micro through hole array template for 3-5 min by using a hydrochloric acid solution with the volume ratio of 0.5% so as to remove processing burrs in the oxide film and the micro through holes; then ultrasonically cleaning the substrate and the micro through hole template for 3-5 min by using acetone, alcohol and deionized water, and removing organic matters on the Cu substrate and the micro through hole array template to obtain a clean Cu substrate and a clean micro through hole array template; then weighing the nano-diamond powder subjected to surface modification by heat treatment, dispersing the nano-diamond powder in deionized water, carrying out ultrasonic treatment for 30-50 min to form a nano-diamond dispersion solution with the concentration of 3.0-7.1 g/ml, immersing a Cu substrate in the prepared nano-diamond dispersion solution, and carrying out ultrasonic oscillation for 10-15 min, so that diamond nano-particles are assembled on the surface of the Cu substrate at the bottom of the micro through hole in an electrostatic manner to serve as seed crystals to induce nucleation and growth rate of diamond in the micro through hole array, and further realizing CVD selective growth of the diamond film; and finally, stacking the micro through hole template on a Cu substrate, and fixing the micro through hole template by using a clamp to prepare for the CVD growth of the diamond film.
Further, the filament is in CH4、H2Keeping the temperature of more than 2500 ℃ for hours in the atmosphere to realize filament carbonization, wherein the total gas flow is 500-600 sccm, CH4The percentage of the carbonization reaction is 3-5%, the air pressure of a reaction chamber is 4.5-5.0 Kpa, and the carbonization reaction is carried out for 2-3 hours fully; then, installing a filament, wherein the filament is a spiral coil, the diameter of the filament is 0.4-0.6 mm, the inner diameter of the spiral is 1-1.5 mm, the number of turns is 12-15, and the distance between two adjacent turns is 0.5-1 mm; then placing the micro-through hole template on a molybdenum support in the reaction cavity, and adjusting the position of the micro-through hole template to align the micro-through hole with the filament; then vacuumizing the cavity, starting an infrared thermometer, and monitoring the temperature of the surface of the micro through hole template; finally using CH4、H2And as a reaction gas, selectively growing a diamond film on the micro-through hole template by CVD.
Further, the technological parameters of the hot wire CVD growth diamond film are as follows: the temperature of the hot wire is 2200 +/-100 ℃, the distance between the hot wire and a substrate is 10 +/-1 mm, the temperature of the substrate is 750 +/-50 ℃, the deposition pressure is 2-3 Kpa, the growth time is 2-3 h, and CH4、H2The total flow rate is 500 to 600sccm,CH4the percentage of the diamond phase is 0.5-3%, the diamond sample crystal grains grown under the process condition are larger, mostly square and triangular, the crystal grains on the surface of the diamond are complete, the shape is regular and the combination is tight, and the diamond phase is good.
Furthermore, the micro-through hole templates are stacked on the Cu substrate, and the diamond film is grown by adopting a template CVD method, so that the selective growth of diamond channels in the micro-through holes can be realized, and in addition, the supporting Cu substrate is easy to peel off.
In conclusion, the heat dissipation effect of the invention is superior to that of traditional heat sink sheets such as Ag, Cu, Al and the like; the heat dissipation performance of the micro-channel Cu-based diamond heat sink sheet is better; the nucleation density and the growth rate of the diamond in the micro through hole are greatly improved; the CVD selective growth of the diamond film is realized in the micro-through hole.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
Fig. 1 is a structural view of a microchannel Cu-based diamond heat sink sheet of the present invention, wherein (a) is a schematic sectional view and (b) is a schematic plan view;
FIG. 2 is a schematic view of a Cu substrate according to the present invention;
FIG. 3 is a schematic diagram of a micro-via template of the present invention, wherein (a) is a schematic cross-sectional view and (b) is a schematic top view;
FIG. 4 is a schematic diagram of nano-diamond particles electrostatically assembled on a metal transition layer on the surface of a Cu substrate according to the present invention;
FIG. 5 is a schematic diagram of a Cu substrate and a micro-via template stack according to the present invention;
FIG. 6 is a schematic diagram of a template CVD process for selectively growing diamond films in accordance with the present invention;
FIG. 7 is a schematic diagram of a diamond micro-channel Cu-based CVD diamond heat sink sheet with a stripped Cu substrate according to the present invention;
FIG. 8 is a schematic view of a diamond micro-channel Cu-based CVD diamond heat sink sheet after chemical mechanical polishing of a diamond surface according to the present invention;
FIG. 9 is a diagram showing the result of numerical simulation of the thermal conductivity of a Cu-based CVD diamond heat sink sheet according to the present invention;
FIG. 10 is a Raman (Roman) spectrum of a diamond microchannel Cu-based CVD diamond heat-sink table diamond of the present invention;
fig. 11 is an electron microscope topography of diamond of the diamond microchannel Cu-based CVD diamond heat sink sheet of the present invention at 50X magnification.
Wherein: a Cu substrate; 2. nano-diamond particles; 3. a micro-via template; CVD diamond is thin.
Detailed Description
Referring to fig. 1 and 2, the invention provides a diamond microchannel Cu-based CVD diamond heat-sink sheet, which sequentially comprises a Cu substrate 1, a micro-via template 3 and a CVD diamond film 4 from bottom to top, wherein nano-diamond particles 2 are arranged between the Cu substrate 1 and the micro-via template 3.
Referring to fig. 2, the Cu substrate 1 is made of oxygen-free copper with a purity of 99.99-99.999%, a diameter of 10-20 mm, and a thickness of 0.5-1 mm.
Referring to fig. 3, a Cu substrate 1 is embedded with a diamond micro-channel array; the diameter of the diamond micro-channel is 0.3-0.5 mm, and the micro-channel interval is 2-3 mm; the diamond microchannel shape includes a circle, a regular triangle, a square, a regular hexagon or a regular octagon. The manufacturing process of the through hole of the diamond micro-channel comprises mechanical punching, hydraulic punching, laser punching and drilling by a drilling machine.
The thickness of the CVD diamond film 4 is 0.2-0.3 mm; the CVD diamond film 4 is selectively grown by adopting a template method CVD; the selective growth is realized by assembling nano diamond particles 2 on the surface of a Cu substrate 1 at the bottom of a micro through hole in an electrostatic manner, and assembling the nano diamond particles 2 on the surface of a micro through hole template 3 without assembling the nano diamond particles 2, wherein the nano diamond particles 2 are spherical, and the average particle size is 2-6 nm, as shown in FIGS. 4 and 5;
CVD includes hot-wire CVD (HFCVD), combustion flame CVD, electron-assisted CVD (EACVD), Microwave Plasma CVD (MPCVD), radio frequency plasma CVD, direct current plasma CVD, hybrid physical chemical vapor CVD (HPCVD), and the like.
The invention relates to a preparation method of a diamond microchannel Cu-based CVD diamond heat-sink sheet, which comprises the following steps:
s1, cutting an oxygen-free copper matrix with the purity of 99.99-99.999% and the diameter of 10-20 mm into a copper sheet with the diameter of 0.5-1 mm as a Cu substrate in a linear mode, and cleaning the surface of the Cu substrate;
s2, manufacturing a micro through hole template, wherein the micro through hole template is made of oxygen-free copper with the same specification as the Cu substrate;
s201, punching a substrate, wherein the micro through hole manufacturing process comprises mechanical punching, hydraulic punching, laser punching, drilling by a drilling machine and the like; the micro through hole template consists of a micro through hole array, the diameter of each micro through hole is 0.3-0.5 mm, and the channel interval is 2-3 mm; the shape of the micro-through hole comprises a circle, a regular triangle, a square, a regular hexagon or a regular octagon, etc., as shown in fig. 5;
s202, slightly corroding the substrate and the micro-through hole template for 3-5 min by using a hydrochloric acid solution with the volume ratio of 0.5%, and removing processing burrs in an oxide film and the micro-through hole;
s203, sequentially using acetone, alcohol and deionized water to ultrasonically clean the substrate and the micro through hole template for 3-5 min, removing organic matters on the surface of the copper sheet, and drying.
S3, assembling nano-diamond particles on the surface of the Cu substrate in an electrostatic manner, and improving the nucleation density of diamond on the gold Cu substrate, wherein the nano-diamond particles are spherical and have an average particle size of 2-6 nm, as shown in figure 4.
The method for selectively growing the diamond film on the micro-through hole template shown in the figure 5 by adopting hot filament CVD mainly comprises the following steps:
s301, immersing a Cu substrate into the prepared nano-diamond dispersion solution, and performing ultrasonic oscillation for 10-15 min;
dispersing the nano-diamond powder subjected to surface modification by heat treatment in deionized water, and carrying out ultrasonic treatment for 30-50 min to form a nano-diamond dispersion solution with the concentration of 3.0-7.1 g/ml;
s302, taking out the Cu substrate, putting the Cu substrate into deionized water to wash away redundant nano diamond particles, and then drying the Cu substrate;
s303, carbonizing filament in CH4、H2Keeping the temperature above 2500 ℃ for a period of time in the atmosphere, the total flow rate of the gas is 500-600 sccm, wherein CH4The percentage of the carbon dioxide is 3-5%, the air pressure of the reaction chamber is 4.5-5.0 Kpa, and the carbon dioxide is fully carbonized for 2-3 hours.
The main purpose of filament carbonization is to prevent the 'pollution' caused by the volatilization of the filament at high temperature, which causes the increase of the non-diamond phase components in the filament and affects the thermal property of the filament;
s304, installing a filament, wherein the filament is a spiral coil made of Ta, W and other materials and used for activating reaction gas, the diameter of the filament is 0.4-0.6 mm, the inner diameter of the spiral is 1-1.5 mm, the number of turns is 12-15, and the distance between every two adjacent turns is 0.5-1 mm;
s305, placing the micro through hole template in the figure 5 on a molybdenum support in a reaction cavity;
s306, adjusting the position of the micro through hole template to align the micro through hole with the filament;
s307, vacuumizing;
s308, starting an infrared thermometer, and monitoring the temperature of the surface of the micro through hole template;
s309 with CH4、H2And as a reaction gas, selectively growing a diamond film on the micro-through hole template by CVD. The main technological parameters are as follows: the hot wire temperature is 2200 +/-100 ℃, the hot wire matrix distance is 10 +/-1 mm, the matrix temperature is 750 +/-50 ℃, the deposition pressure is 2-3 Kpa, the growth time is 2-3 h, and CH4、H2A total flow rate of 500 to 600sccm, wherein CH4The percentage of (A) is 0.5% -3%;
and S310, characterizing and analyzing the sample by using a Raman (Roman) spectrometer and an electron microscope.
S4, stacking the micro-through-hole template on a Cu substrate, fixing the micro-through-hole template by using a clamp, and selectively growing a diamond film by adopting a template method CVD, wherein the thickness of the CVD diamond film is 0.2-0.3 mm;
the CVD diamond film growth method comprises Hot Filament CVD (HFCVD), combustion flame CVD, Electron Assisted CVD (EACVD), Microwave Plasma CVD (MPCVD), radio frequency plasma CVD, direct current plasma CVD, mixed physical chemical vapor CVD (HPCVD), etc.;
s5, chemically and mechanically polishing the diamond surface to enable the diamond on the surface to be flat;
s6, peeling the Cu substrate, and slightly prying the Cu substrate along the gap between the Cu substrate and the micro through hole template by using a pair of tweezers to remove the Cu substrate; or soaking the sample in a ferric trichloride solution for 30-60 s to remove the Cu substrate, as shown in FIG. 7.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
S1, cutting an oxygen-free copper matrix with the purity of 99.99% and the diameter of 10mm into a copper sheet with the diameter of 0.5mm as a Cu substrate in a linear manner, and cleaning the surface of the Cu substrate;
s201, punching and punching a Cu substrate, wherein the micro through hole manufacturing process comprises mechanical punching and punching, hydraulic punching, laser punching, drilling by a drilling machine and the like; the micro through hole template consists of a micro through hole array, the diameter of each micro through hole is 0.3mm, and the channel spacing is 2 mm; the shape of the micro through hole comprises a circle, a regular triangle, a square, a regular hexagon or a regular octagon;
s202, slightly corroding the Cu substrate and the micro through hole template for 3min by using a hydrochloric acid solution with the volume ratio of 0.5%, and removing processing burrs in an oxide film and the micro through holes;
s203, sequentially using acetone, alcohol and deionized water to ultrasonically clean the substrate and the micro through hole template for 3min, removing organic matters on the surface of the copper sheet, and drying;
s204, weighing 3g of the nano-diamond powder subjected to heat treatment surface modification, dispersing in 70ml of deionized water, and performing ultrasonic treatment for 30min to form a nano-diamond dispersion solution; immersing a Cu substrate into the prepared nano-diamond dispersion solution, and carrying out ultrasonic oscillation for 10 min;
s205, taking out the Cu substrate, putting the Cu substrate into deionized water to wash away redundant nano diamond particles, and then drying the Cu substrate;
and S206, stacking the micro through hole template on the Cu substrate and fixing the micro through hole template by using a clamp.
S3, assembling nano diamond particles on the surface of the Cu substrate in an electrostatic manner, and improving the nucleation density of diamond on the gold Cu substrate, wherein the nano diamond particles are spherical and have the average particle size of 2 nm; the method comprises the following steps:
s301, carbonizing filament in CH4、H2Keeping the temperature above 2500 ℃ for hours in the atmosphere, wherein the total flow of the gas is 500sccm and CH4The percentage of the carbon dioxide is 3 percent, the air pressure of a reaction chamber is 4.5Kpa, and the carbon dioxide is fully carbonized for 2 hours;
the main purpose of filament carbonization is to prevent the 'pollution' caused by the volatilization of the filament at high temperature, which causes the increase of the non-diamond phase components in the filament and affects the thermal property of the filament;
s302, installing a filament, wherein the filament is a spiral coil made of Ta, W and other materials and used for activating reaction gas, the diameter of the filament is 0.4mm, the inner diameter of the spiral is 1mm, the number of turns is 12, and the distance between two adjacent turns is 0.5 mm;
s303, placing the micro through hole template on a molybdenum support in the reaction cavity;
s304, adjusting the position of the micro through hole template to align the micro through hole with the filament;
s305, vacuumizing;
s306, starting an infrared thermometer, and monitoring the temperature of the surface of the micro through hole template;
s307, with CH4、H2And as a reaction gas, selectively growing a diamond film on the micro-through hole template by CVD. The main technological parameters are as follows: the temperature of the hot wire is 2200 +/-100 ℃, the distance between the hot wire and the matrix is 10 +/-1 mm, the temperature of the matrix is 750 +/-50 ℃, the deposition pressure is 2Kpa, the growth time is 2h, and CH4、H2Total flow rate 500sccm, where, CH4The percentage of (A) is 0.5%;
and S308, characterizing and analyzing the sample by using a Raman (Roman) spectrometer and an electron microscope.
S4, stacking the micro through hole templates on a Cu substrate, and selectively growing a diamond film by adopting a template method CVD, wherein the thickness of the CVD diamond film is 0.2 mm;
s5, chemically and mechanically polishing the diamond surface to enable the diamond on the surface to be flat;
s6, peeling the Cu substrate, and slightly prying the Cu substrate along the gap between the Cu substrate and the micro through hole template by using a pair of tweezers to remove the Cu substrate; or soaking the sample in a ferric trichloride solution for 30s to remove the Cu substrate.
Example 2
S1, cutting an oxygen-free copper matrix with the purity of 99.99 percent and the diameter of 14mm into a copper sheet with the diameter of 0.7mm as a Cu substrate in a linear manner, and cleaning the surface of the Cu substrate;
s201, punching and punching a Cu substrate, wherein the micro through hole manufacturing process comprises mechanical punching and punching, hydraulic punching, laser punching, drilling by a drilling machine and the like; the micro through hole template consists of a micro through hole array, the diameter of each micro through hole is 0.4mm, and the channel spacing is 2 mm; the shape of the micro through hole comprises a circle, a regular triangle, a square, a regular hexagon or a regular octagon;
s202, slightly corroding the Cu substrate and the micro through hole template for 4min by using a hydrochloric acid solution with the volume ratio of 0.5%, and removing processing burrs in an oxide film and the micro through holes;
s203, sequentially using acetone, alcohol and deionized water to ultrasonically clean the substrate and the micro through hole template for 4min, removing organic matters on the surface of the copper sheet, and drying;
s204, weighing 4g of the nano-diamond powder subjected to heat treatment surface modification, dispersing the nano-diamond powder in 80ml of deionized water, and performing ultrasonic treatment for 40min to form a nano-diamond dispersion solution; immersing a Cu substrate into the prepared nano-diamond dispersion solution, and carrying out ultrasonic oscillation for 12 min;
s205, taking out the Cu substrate, putting the Cu substrate into deionized water to wash away redundant nano diamond particles, and then drying the Cu substrate;
and S206, stacking the micro through hole template on the Cu substrate and fixing the micro through hole template by using a clamp.
S3, assembling nano diamond particles on the surface of the Cu substrate in an electrostatic manner, and improving the nucleation density of diamond on the gold Cu substrate, wherein the nano diamond particles are spherical and have an average particle size of 4 nm; the method comprises the following steps:
s301, carbonizing filament in CH4、H2Keeping the temperature above 2500 ℃ for hours in the atmosphere, wherein the total flow of the gas is 550sccm and CH4The percentage of the carbon dioxide is 4 percent, the air pressure of a reaction chamber is 4.7Kpa, and the carbon dioxide is fully carbonized for 2.5 hours;
the main purpose of filament carbonization is to prevent the 'pollution' caused by the volatilization of the filament at high temperature, which causes the increase of the non-diamond phase components in the filament and affects the thermal property of the filament;
s302, installing a filament, wherein the filament is a spiral coil made of Ta, W and other materials and used for activating reaction gas, the diameter of the filament is 0.5mm, the inner diameter of the spiral is 1.2mm, the number of turns is 13, and the distance between two adjacent turns is 0.7 mm;
s303, placing the micro through hole template on a molybdenum support in the reaction cavity;
s304, adjusting the position of the micro through hole template to align the micro through hole with the filament;
s305, vacuumizing;
s306, starting an infrared thermometer, and monitoring the temperature of the surface of the micro through hole template;
s307, with CH4、H2And as a reaction gas, selectively growing a diamond film on the micro-through hole template by CVD. The main technological parameters are as follows: the temperature of the hot wire is 2200 +/-100 ℃, the distance between the hot wire and the matrix is 10 +/-1 mm, the temperature of the matrix is 750 +/-50 ℃, the deposition pressure is 2.5Kpa, the growth time is 2.5h, and CH4、H2Total flow rate 550sccm, where CH4The percentage of (A) is 1.5%;
and S308, characterizing and analyzing the sample by using a Raman (Roman) spectrometer and an electron microscope.
S4, stacking the micro through hole templates on a Cu substrate, and selectively growing a diamond film by adopting a template method CVD, wherein the thickness of the CVD diamond film is 0.2 mm;
s5, chemically and mechanically polishing the diamond surface to enable the diamond on the surface to be flat;
s6, peeling the Cu substrate, and slightly prying the Cu substrate along the gap between the Cu substrate and the micro through hole template by using a pair of tweezers to remove the Cu substrate; or soaking the sample in a ferric trichloride solution for 40s to remove the Cu substrate.
Example 3
S1, cutting an oxygen-free copper matrix with the purity of 99.999% and the diameter of 18mm into a copper sheet with the diameter of 0.9mm as a Cu substrate in a linear mode, and cleaning the surface of the Cu substrate;
s201, punching and punching a Cu substrate, wherein the micro through hole manufacturing process comprises mechanical punching and punching, hydraulic punching, laser punching, drilling by a drilling machine and the like; the micro through hole template consists of a micro through hole array, the diameter of each micro through hole is 0.4mm, and the channel spacing is 3 mm; the shape of the micro through hole comprises a circle, a regular triangle, a square, a regular hexagon or a regular octagon;
s202, slightly corroding the Cu substrate and the micro through hole template for 4min by using a hydrochloric acid solution with the volume ratio of 0.5%, and removing processing burrs in an oxide film and the micro through holes;
s203, sequentially using acetone, alcohol and deionized water to ultrasonically clean the substrate and the micro through hole template for 4min, removing organic matters on the surface of the copper sheet, and drying;
s204, weighing 4g of the nano-diamond powder subjected to heat treatment surface modification, dispersing in 90ml of deionized water, and performing ultrasonic treatment for 45min to form a nano-diamond dispersion solution; immersing a Cu substrate into the prepared nano-diamond dispersion solution, and carrying out ultrasonic oscillation for 14 min;
s205, taking out the Cu substrate, putting the Cu substrate into deionized water to wash away redundant nano diamond particles, and then drying the Cu substrate;
and S206, stacking the micro through hole template on the Cu substrate and fixing the micro through hole template by using a clamp.
S3, assembling nano diamond particles on the surface of the Cu substrate in an electrostatic manner, and improving the nucleation density of diamond on the gold Cu substrate, wherein the nano diamond particles are spherical and have the average particle size of 5 nm; the method comprises the following steps:
s301, carbonizing filament in CH4、H2Keeping the temperature above 2500 ℃ for hours in the atmosphere, and keeping the total flow of the gas at 580sccm and CH4The percentage of the carbon dioxide is 4 percent, the air pressure of a reaction chamber is 4.9Kpa, and the carbon dioxide is fully carbonized for 2.5 hours;
the main purpose of filament carbonization is to prevent the 'pollution' caused by the volatilization of the filament at high temperature, which causes the increase of the non-diamond phase components in the filament and affects the thermal property of the filament;
s302, installing a filament, wherein the filament is a spiral coil made of Ta, W and other materials and used for activating reaction gas, the diameter of the filament is 0.5mm, the inner diameter of the spiral is 1.4mm, the number of turns is 14, and the distance between two adjacent turns is 0.9 mm;
s303, placing the micro through hole template on a molybdenum support in the reaction cavity;
s304, adjusting the position of the micro through hole template to align the micro through hole with the filament;
s305, vacuumizing;
s306, starting an infrared thermometer, and monitoring the temperature of the surface of the micro through hole template;
s307, with CH4、H2And as a reaction gas, selectively growing a diamond film on the micro-through hole template by CVD. The main technological parameters are as follows: the temperature of the hot wire is 2200 +/-100 ℃, the distance between the hot wire and the matrix is 10 +/-1 mm, the temperature of the matrix is 750 +/-50 ℃, the deposition pressure is 2.5Kpa, the growth time is 2.5h, and CH4、H2Total flow rate 580sccm where, CH4The percentage of (A) is 2.5%;
and S308, characterizing and analyzing the sample by using a Raman (Roman) spectrometer and an electron microscope.
S4, stacking the micro through hole templates on a Cu substrate, and selectively growing a diamond film by adopting a template method CVD, wherein the thickness of the CVD diamond film is 0.3 mm;
s5, chemically and mechanically polishing the diamond surface to enable the diamond on the surface to be flat;
s6, peeling the Cu substrate, and slightly prying the Cu substrate along the gap between the Cu substrate and the micro through hole template by using a pair of tweezers to remove the Cu substrate; or soaking the sample in a ferric trichloride solution for 50s to remove the Cu substrate.
Example 4
S1, cutting an oxygen-free copper matrix with the purity of 99.999% and the diameter of 20mm into a copper sheet with the diameter of 1mm as a Cu substrate in a linear mode, and cleaning the surface of the Cu substrate;
s201, punching and punching a Cu substrate, wherein the micro through hole manufacturing process comprises mechanical punching and punching, hydraulic punching, laser punching, drilling by a drilling machine and the like; the micro through hole template consists of a micro through hole array, the diameter of each micro through hole is 0.5mm, and the channel spacing is 3 mm; the shape of the micro through hole comprises a circle, a regular triangle, a square, a regular hexagon or a regular octagon;
s202, slightly corroding the Cu substrate and the micro through hole template for 5min by using a hydrochloric acid solution with the volume ratio of 0.5%, and removing processing burrs in an oxide film and the micro through holes;
s203, sequentially using acetone, alcohol and deionized water to ultrasonically clean the substrate and the micro through hole template for 5min, removing organic matters on the surface of the copper sheet, and drying;
s204, weighing 5g of the nano-diamond powder subjected to heat treatment surface modification, dispersing the nano-diamond powder in 100ml of deionized water, and performing ultrasonic treatment for 50min to form a nano-diamond dispersion solution; immersing a Cu substrate into the prepared nano-diamond dispersion solution, and carrying out ultrasonic oscillation for 15 min;
s205, taking out the Cu substrate, putting the Cu substrate into deionized water to wash away redundant nano diamond particles, and then drying the Cu substrate;
and S206, stacking the micro through hole template on the Cu substrate and fixing the micro through hole template by using a clamp.
S3, assembling nano diamond particles on the surface of the Cu substrate in an electrostatic manner, and improving the nucleation density of diamond on the gold Cu substrate, wherein the nano diamond particles are spherical and have an average particle size of 6 nm; the method comprises the following steps:
s301, carbonizing filament in CH4、H2Keeping the temperature above 2500 ℃ for hours in the atmosphere, wherein the total flow of the gas is 600sccm and CH4The percentage of the carbon dioxide is 5 percent, the air pressure of a reaction chamber is 5.0Kpa, and the carbon dioxide is fully carbonized for 3 hours;
the main purpose of filament carbonization is to prevent the 'pollution' caused by the volatilization of the filament at high temperature, which causes the increase of the non-diamond phase components in the filament and affects the thermal property of the filament;
s302, installing a filament, wherein the filament is a spiral coil made of Ta, W and other materials and used for activating reaction gas, the diameter of the filament is 0.6mm, the inner diameter of the spiral is 1.5mm, the number of turns is 15, and the distance between two adjacent turns is 1 mm;
s303, placing the micro through hole template on a molybdenum support in the reaction cavity;
s304, adjusting the position of the micro through hole template to align the micro through hole with the filament;
s305, vacuumizing;
s306, starting an infrared thermometer, and monitoring the temperature of the surface of the micro through hole template;
s307, with CH4、H2And as a reaction gas, selectively growing a diamond film on the micro-through hole template by CVD. The main technological parameters are as follows: the temperature of the hot wire is 2200 +/-100 ℃, the distance between the hot wire and a matrix is 10 +/-1 mm, the temperature of the matrix is 750 +/-50 ℃, the deposition pressure is 3Kpa, the growth time is 3h, and CH4、H2Total flow rate 600sccm, where CH4The percentage of (A) is 3%;
and S308, characterizing and analyzing the sample by using a Raman (Roman) spectrometer and an electron microscope.
S4, stacking the micro through hole templates on a Cu substrate, and selectively growing a diamond film by adopting a template method CVD, wherein the thickness of the CVD diamond film is 0.3 mm;
s5, chemically and mechanically polishing the diamond surface to enable the diamond on the surface to be flat;
s6, peeling the Cu substrate, and slightly prying the Cu substrate along the gap between the Cu substrate and the micro through hole template by using a pair of tweezers to remove the Cu substrate; or soaking the sample in a ferric trichloride solution for 60s to remove the Cu substrate.
Compared with the prior art, the invention has the advantages that:
(1) according to the method, the diamond with high thermal conductivity is used as the heat sink, and the heat dissipation effect is superior to that of traditional heat sink sheets such as Ag, Cu and Al.
(2) Compared with the traditional Cu-based diamond film heat sink sheet with the serial structure of the upper layer and the lower layer, the micro-channel Cu-based diamond heat sink sheet forms a longitudinal diamond heat dissipation channel on the Cu substrate, so that the problem of limitation of large heat groups of the Cu substrate on the heat dissipation performance of the heat sink sheet is solved; compared with a diamond powder particle/copper composite heat sink sheet, the micro-channel Cu-based diamond heat sink sheet has the advantages that a continuous diamond heat dissipation channel is formed on the Cu substrate, the problem of limitation on heat dissipation performance of the heat sink sheet caused by continuous distribution of diamond powder particles in Cu is solved, and the heat dissipation performance of the micro-channel Cu-based diamond heat sink sheet is better.
(3) Diamond nano particles are assembled on the surface of the Cu substrate at the bottom of the micro through hole in an electrostatic manner, so that the nucleation density and the growth rate of diamond in the micro through hole are greatly improved; and the nucleation density and the growth rate of diamond on the surface of the untreated micro-through hole template are low, and the CVD selective growth of the diamond film is realized in the micro-through hole.
Referring to fig. 9, it can be seen that the diamond surface and tangential temperature gradient is obvious, the isotherm is clear, and the surface of the present invention has good thermal conductivity.
Referring to FIG. 10, it can be seen that the peak is at 1350cm-1The Raman scattering characteristic peak of the polycrystalline diamond indicates that the grown diamond is polycrystalline.
Referring to fig. 11, it can be seen that the diamond sample shows that the grains are larger, mostly square and triangular, the surface grains of the diamond are complete, the shape is regular and the bonding is tight, and the diamond phase is good.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (1)
1. A preparation method of a diamond micro-channel Cu-based CVD diamond heat-sink sheet is characterized by comprising the following steps:
s1, cutting an oxygen-free copper wire with the purity of 99.99-99.999% and the diameter of 10-20 mm into a copper sheet with the diameter of 0.5-1 mm as a Cu substrate, and cleaning the surface of the Cu substrate;
s2, manufacturing a micro through hole template, wherein the micro through hole template is made of oxygen-free copper with the same specification as the Cu substrate, and the step S2 specifically comprises the following steps:
s201, punching and punching the oxygen-free copper by adopting a mechanical punching and punching, hydraulic punching, laser punching or drilling machine drilling process, wherein the diameter of the micro through holes is 0.3-0.5 mm, and the distance between the micro through holes is 2-3 mm; the shape of the micro through hole comprises a circle, a regular triangle, a square, a regular hexagon or a regular octagon;
s202, slightly corroding the micro-through hole template for 3-5 min by using a hydrochloric acid solution with the volume ratio of 0.5%, and removing an oxide film and processing burrs in the micro-through hole;
s203, ultrasonically cleaning the micro-through hole template for 3-5 min by sequentially using acetone, alcohol and deionized water, removing organic matters on the surface of the micro-through hole template, and drying;
s3, assembling nano-diamond particles on the surface of the Cu substrate in a static manner, improving the nucleation density of diamond on the Cu substrate, wherein the nano-diamond particles are spherical, and have an average particle size of 2-6 nm, and specifically comprise the following steps: dispersing the nano-diamond powder subjected to surface modification by heat treatment in deionized water, performing ultrasonic treatment for 30-50 min to form a nano-diamond dispersion solution with the concentration of 3.0-7.1 g/ml, immersing a Cu substrate in the prepared nano-diamond dispersion solution, and performing ultrasonic oscillation for 10-15 min; taking out the Cu substrate, putting the Cu substrate into deionized water to wash away redundant nano diamond particles, and drying the micro through hole template;
s4, stacking the micro-through-hole template on a Cu substrate, fixing the micro-through-hole template by using a clamp, and selectively growing a diamond film by adopting a template method CVD, wherein the thickness of the CVD diamond film is 0.2-0.3 mm, and the method specifically comprises the following steps:
carbonizing a front filament of a growing diamond film by CVD, keeping the temperature of the front filament to be higher than 2500 ℃ in an atmosphere of CH4 and H2, fully carbonizing the front filament for 2-3 hours, wherein the total gas flow is 500-600 sccm, the percentage of CH4 is 3-5%, and the air pressure of a reaction chamber is 4.5-5.0 Kpa;
installing a filament, wherein the filament is a spiral coil, the diameter of the filament is 0.4-0.6 mm, the inner diameter of the spiral is 1-1.5 mm, the number of turns is 12-15, and the distance between two adjacent turns is 0.5-1 mm; placing the micro-through hole template on a molybdenum support in a reaction cavity; adjusting the position of the micro-through hole template to align the micro-through hole with the filament; vacuumizing; starting an infrared thermometer, and monitoring the temperature of the surface of the micro through hole template; using CH4 and H2 as reaction gases, and selectively growing a diamond film on the micro through hole template by CVD;
the CVD selective growth diamond film comprises the following specific steps: the filament temperature is 2200 +/-100 ℃, the distance between the filament and the Cu substrate is 10 +/-1 mm, the Cu substrate temperature is 750 +/-50 ℃, the deposition pressure is 2-3 Kpa, the growth time is 2-3H, the total flow of CH4 and H2 is 500-600 sccm, and the percentage of CH4 is 0.5% -3%;
s5, polishing the diamond film by adopting chemical machinery;
s6, peeling the Cu substrate, and prying the Cu substrate along a gap between the Cu substrate and the micro through hole template to remove the Cu substrate; or soaking the sample in a ferric trichloride solution for 30-60 s to remove the Cu substrate.
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| CN107845616A (en) * | 2017-11-09 | 2018-03-27 | 青岛理工大学 | Nested type super-high heat-conductive diamond film/silicon based composite material and preparation method thereof |
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| CN107845616A (en) * | 2017-11-09 | 2018-03-27 | 青岛理工大学 | Nested type super-high heat-conductive diamond film/silicon based composite material and preparation method thereof |
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