CN108682662B - Preparation method of diamond micro-channel heat sink for heat dissipation with ultrahigh heat flow density - Google Patents
Preparation method of diamond micro-channel heat sink for heat dissipation with ultrahigh heat flow density Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
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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
- C23C16/27—Diamond only
- C23C16/276—Diamond only using plasma jets
Abstract
The invention relates to a preparation method of a diamond micro-channel heat sink for heat dissipation with ultrahigh heat flow density, belonging to the field of heat dissipation of semiconductor devices. The preparation of the high-quality, crack-free and super-thick diamond self-supporting film is realized through a special substrate technology and an improved CVD (chemical vapor deposition) preparation process; controlling the surface roughness of the diamond super-thick film by mechanical grinding and polishing according to the requirement of a thermal contact interface; and then, the structural size of the diamond ultra-thick film is shaped by adopting a unique laser processing technology, and microgroove carving is carried out on the surface by utilizing laser microgeam to obtain the diamond microchannel heat exchanger with qualified size and groove shape, so that the diamond microchannel heat exchanger meets the design requirement of a heat exchanger for dissipating high heat flux density. The microchannel heat sink can be used for heat dissipation of high-power-consumption electronic devices of space loads such as phased array radars, satellites and large-scale spacecrafts.
Description
Technical Field
The invention belongs to the field of heat dissipation of electronic devices with high heat flux density, and particularly provides a preparation method of a diamond microchannel heat sink for heat dissipation with ultrahigh heat flux density.
Background
With the continuous improvement of the functions and the operation speed of electronic devices and the acceleration of the trend of miniaturization and integration of the devices, the heat flux density generated during the operation of the electronic devices rapidly rises. The reliability of the working performance of the device is seriously influenced by the heating problem of the device, and researches show that the reliability is reduced by 5 percent when the temperature of the device is increased by 1 ℃ at the level of 70-80 ℃. In advanced devices such as high-power communication and navigation satellites, directional high-energy weapons, wide-bandgap semiconductor radars and the like which are developed at present, the unit heat flux density of core electronic devices is up to hundreds of watts or even kilowatts. This high heat must be dissipated in a timely manner or it can affect the performance and useful life of the device.
The micro-channel heat dissipation loop is a good heat control technology for dissipating high heat flow density, the core component of the micro-channel heat exchanger is characterized by high aspect ratio, a large amount of heat can be taken away only by small volume, the requirement on temperature uniformity can be well met, and the micro-channel heat dissipation loop is very suitable for occasions with large heat dissipation capacity and strict space requirement.
The microchannel materials commonly used at present are mostly metallic materials (e.g., Cu) and semiconductor materials (e.g., Si). The heat conductivity of the silicon material is greatly changed along with the temperature, the heat conductivity is 153.5W/(m.K) at 27 ℃, the heat conductivity is reduced to 113.7W/(m.K) at 100 ℃, the capability of dissipating high heat flux density is insufficient, and the requirement on equipment is high and the welding process is complex when a silicon micro-channel structure is processed. Although the copper micro-channel structure has high thermal conductivity (398W/m.K), the machining method based on engraving and washing has processing shear stress, cannot meet the processing requirement of a thin channel wall, and is difficult to realize a high aspect ratio structure, so the heat dissipation effect is not ideal. Diamond is a material with the highest known thermal conductivity in nature, has very stable physical and chemical inertness and extremely high mechanical strength and electrical insulation, and is an ideal material for manufacturing the micro-channel heat exchanger. However, the CVD diamond film required to fabricate the microchannels must be of sufficient thickness (typically above 3 mm), which is extremely challenging with the CVD techniques currently employed to deposit diamond films. In addition, the special physical and chemical properties of diamond material make it very difficult to precisely micro-groove and only by using a unique laser engraving process.
Disclosure of Invention
The invention aims to solve the problems that: according to the design requirements of the current thermal management system for the ultrahigh heat flow density device, a process for obtaining the ultra-thick diamond film is provided, and a method for preparing the microchannel heat sink based on the ultra-thick diamond film solves the problem of ultrahigh heat flow density dissipation of the high-power electronic device. The thermal conductivity of diamond is as high as 2000W/m.K, and the diamond can achieve excellent heat dissipation effect by combining with a micro-channel design with a high aspect ratio. Firstly, a direct current arc plasma jet CVD system is adopted, and multiple re-nucleation is promoted by adjusting process parameters in stages, so that uniform and compact deposition of a large-area diamond super-thick film is realized. The mechanical grinding and polishing technology is adopted, and the protrusions on the surface of the diamond film are removed based on the grinding action of the diamond powder, so that the surface of the diamond thick film is flattened; and then, precisely etching the surface of the diamond by adopting laser, and adjusting the convergence angle of the laser beam to form a high-aspect-ratio micro-channel with a specific section shape.
A preparation method of diamond micro-channel heat sink for heat dissipation with ultrahigh heat flow density is characterized in that the preparation of an ultra-thick diamond film is realized through an improved direct current jet CVD process, then a micro-flow channel is laser engraved on the surface of the diamond ultra-thick film and used for a pump-driven heat transfer fluid loop, the heat dissipation and the high-efficiency heat transfer of diamond can be realized at the same time, and the heat dissipation with ultrahigh heat flow density is realized, and the preparation method specifically comprises the following steps:
step 1: preparing an ultra-thick CVD diamond film;
1.1 selecting high-temperature molybdenum as a diamond thick film deposition substrate, and plating a composite transition layer on the surface of the molybdenum substrate in advance to reduce the thermal stress concentration in the deposition process and improve the demoulding yield.
1.2 placing the processed substrate into a high-energy activation plasma chamber to prepare a diamond super-thick film, setting an initial deposition process, increasing the concentration of methane by 20-50sccm on the basis of growth flow at intervals of 50-100 hours, increasing the concentration of high-energy carbon atom groups for a short time to realize secondary nucleation, closing the methane after 10-25min, then etching by using hydrogen/argon plasma for 5-10min to remove a formed non-diamond phase, and then adjusting the concentration of the methane back to the growth concentration. The total deposition time is 300-600 h, and a diamond thick film with the thickness of about 4-6mm is obtained.
Step 2: grinding and polishing the diamond thick film;
in order to meet the requirement of welding the subsequent microchannel heat sink and the heat source surface, improve the flatness and reduce the interface thermal resistance, the obtained diamond thick film is polished by a grinding polisher until the surface roughness reaches 0.5-3.2 mu m. In view of the longer polishing time of the diamond thick film, the grinding and polishing adopts an automatic powder adding device (patent ZL201310150661.8) so as to save labor and facilitate operation.
And step 3: forming the structure of the diamond thick film;
in order to obtain the diamond heat sink which meets the structure size, the diamond film needs to be cut by high-energy laser beams. The diamond thick film has large internal stress, and the diamond thick film is easy to crack randomly in the cutting process due to the thermal stress concentration generated in the laser forming process. Therefore, at the beginning of laser processing, a low power, low rate laser cutting process is employed. The laser is a YAG laser generator (special for diamond) with laser wavelength of 1064 nm.
And 4, step 4: constructing a microfluidic channel on the surface of the diamond film by laser cutting;
and similarly, a microfluidic channel is constructed on the surface of the diamond thick film by using the laser micro-beam, and a high-aspect-ratio structure and good surface quality are obtained by accurately controlling parameters such as laser spot size, focusing depth, beam convergence angle, cutting frequency, cutting rate and the like. In order to obtain a specific micro-groove section shape, the inclined height of the sample stage in the X-Y direction is adjusted, or the opening angle of a laser beam is adjusted in a small range.
Furthermore, the thickness of the ultra-thick diamond film in a deposition state is more than or equal to 4mm, and the thickness of the micro-groove after processing is more than or equal to 3 mm.
Furthermore, a high-temperature molybdenum material of a pre-plated composite transition layer is used as a substrate, and the composite transition layer is made of Ti, Mo, Si or W. The ultra-thick diamond film is prepared by adopting a direct current jet CVD method with an improved process.
Further, the direct current injection CVD method of the improved process is characterized in that: intermittently adjusting the secondary nucleation process and assisting in H2the/Ar plasma processing technology realizes secondary re-nucleation, inhibits the abnormal growth of large columnar crystals, and improves the grain density of the diamond film, thereby ensuring that the effective growth thickness of the diamond thick film reaches more than 4 mm.
Further, the micro-channel heat exchanger is characterized in that: the micro-channel heat exchanger is made of full diamond materials, and the thickness dimension of the micro-channel is larger than 3 mm.
Further, the micro-channel heat exchanger is characterized in that: the shaping of the diamond is realized by adopting a special laser cutting machine for the diamond; and processing of different groove types is realized by adjusting the deflection angle of the X-Y axis of the laser and the opening angle of the laser.
Further, the microgroove heat exchanger is characterized in that: the roughness control of the thermal contact surface is realized by a mechanical grinding technology, so that the welding strength and the thermal resistance minimum effect are met, and the roughness is 0.5-3.2 mu m.
Therefore, the microfluidic channel is constructed on the diamond ultra-thick film to greatly improve the heat dissipation capacity of the high-power device, and the heat dissipation requirement of the electronic equipment with ultra-high heat flow density can be met.
The key of the implementation process of the invention is as follows:
1. the design of the substrate material and the transition layer is very critical for obtaining a crack-free high-strength diamond thick film. The invention adopts the composite transition layer plated on the high-temperature molybdenum substrate, and carries out composite matching on materials such as Ti, W, Mo, Si and the like, thereby not only realizing good stress transition in the deposition process of the high-thickness diamond film, but also playing a good stress release role in the shrinkage demoulding process in the cooling process.
2. Multiple re-nucleation technology is adopted in the growth process, the methane flow is adjusted up in a short time, the concentration of high-energy atomic groups is increased, the re-nucleation density of diamond is improved, the defect of pores generated by columnar crystal growth in the growth process of the diamond film is filled, and the defect of pores generated by columnar crystal growth can be restrainedThe transverse growth of large crystal grains is realized, so that the size of the crystal grains is relatively small, and the dense and uniform growth of the high-thickness diamond film is realized. At the same time, with H2And the/Ar plasma processing technology is used for etching the non-diamond phase generated in the secondary nucleation process, so that the final quality of the CVD diamond thick film is ensured.
3. The cross-sectional shapes of the micro-channels are different, the flow pattern of the heat transfer fluid in the channels is different, and the heat transfer fluid is subjected to different corner effects and different collision and disturbance among the fluids, so that the heat dissipation capacity of the system is different. If a V-shaped groove, a U-shaped groove or a trapezoidal groove is to be obtained, the cutting adjustment can be realized by the following cutting adjustment modes: (1) the cutting line moves left and right for a very small distance to sweep to change the gradient and the width of the micro-groove after cutting, (2) the inclination angle of the sample stage in the X-Y direction is adjusted in the cutting process, and (3) the opening angle of a laser beam is reduced along with the increase of the cutting depth in the cutting process, wherein the adjustment range is 6-14 degrees.
The invention has the advantages that:
the prepared diamond film has large thickness and high quality, and meets the requirements of micro-groove processing; the diamond micro-channel has strong heat exchange capability, is convenient for structural layout, is easy to organize internal heat exchange, is safe and reliable, is an active heat control technology with high reliability, can obtain good temperature control effect, and has wide application prospect particularly on large-scale spacecrafts.
1. The diamond super-thick film with the thickness of about 4-6mm is prepared by combining multiple re-nucleation technology in the growth process and adjusting the methane growth flow by stages, is a CVD diamond film with the highest thickness known at home and abroad at present, and has uniform and compact thick film, good surface quality and good performance.
2. The micro-channel is processed by laser, and the micro-groove obtained after the selection process has high dimensional precision and good shape and is convenient for structural layout in a system. Micro-channels with different cross-sectional shapes can be formed by adjusting laser cutting parameters, a high aspect ratio structure can be obtained, and the contact area of the heat transfer working medium and the micro-channels is increased.
3. The diamond has excellent heat conducting performance, and the diamond super-thick film with high heat conducting performance is combined with the flowing boiling of the heat transfer fluid in the micro-channel with high aspect ratioGreatly optimizes the heat transfer performance, and the heat exchange capacity is as high as 1000W/cm2The heat dissipation material is far higher than other heat dissipation materials, and the heat dissipation requirement of high-power-consumption electronic equipment is met.
4. The chemical property of diamond is stable, acid and alkali resistance and corrosion resistance, so that the heat transfer working medium range of the diamond micro-channel heat sink can be wider. The diamond has small thermal expansion coefficient and safe and reliable performance, and can not be obviously changed after long-term use.
Detailed Description
The technical scheme of the invention is further explained by combining the specific embodiment as follows:
the molybdenum substrate after grinding and cleaning uses a direct current plasma jet chemical vapor deposition device to grow the diamond ultra-thick film, the substrate is placed on a deposition table, the vacuum degree of a deposition chamber is pumped to be below 0.1Pa by a pump set, and H is introduced2After igniting the arc with Ar, introducing CH4Gas, the diamond film begins to deposit.
Example 1
Growing a diamond ultra-thick film on a high-temperature molybdenum substrate by adopting a CVD method, and plating a composite transition layer on the molybdenum substrate, wherein the substrate has the following dimensions: the diameter is 100mm, and the thickness is 50 mm. Substrate processing parameters: grinding with diamond paste with particle size of 0.5 μm for 5min, and washing with acetone for 2 times. Deposition parameters of the diamond film: the deposition temperature is 880 ℃, the distance between the substrate and the anode is 1cm, the deposition pressure is 3.0Kpa, the cooling water temperature is less than or equal to 25 ℃, the Ar flow is 4.0SLM, H2Flow rate of 7.8SLM, CH4The flow is 110SCCM, and each 100h of growth, CH is added4Flow Up to 130SCCM, Re-nucleation for 10min, followed by CH shut-off4Hold H2And performing/Ar plasma treatment for 10 min. Then setting CH4The flow to 110SCCM continues to grow for 100 h. Until the deposition time is 450h, finally obtaining the diamond thick film with the thickness of 4 mm. And grinding and polishing the surface of the diamond film by using a grinding and polishing machine, wherein the thickness of the polished diamond film is 3 mm. The polishing parameters were: the diamond abrasive particle size is selected to be 100#, the rotating speed of the grinding disc is 80rmp, and the loading weight is 400 g. And cutting a structure with the size of 25mm multiplied by 10mm on the diamond thick film by using a laser cutter, wherein the cutting parameters of the laser are as follows: has a power of80W, the sample feeding speed is 150mm/min, and the cutting times are 10 times. And the laser program is set to sweep once on the cutting line, then sweep once along a straight line after moving 0.02mm to the left side of the cutting line, then sweep once along a straight line after moving 0.02mm to the right side of the cutting line, and finally obtain the required diamond structure after multiple cycles. Further adopting laser high-energy beam to construct a micro-channel on the surface of the diamond, wherein the width of the micro-channel is 0.2mm, the depth is 1mm, and the cutting parameters are as follows: the power was 80W, the sample feed rate was 100mm/min, and the initial laser beam angle was 14 °. Reducing the opening angle of the laser beam by 1 degree once per cycle, completing the cutting after the program is cycled for 8 times, and pickling the sample to remove the graphite and other impurities remained on the surface after the laser cutting. Finally obtaining the diamond micro-channel heat sink structure, wherein the thermal conductivity of the diamond thick film is 1500W/mK through measurement. Liquid ammonia is used as a cooling medium, 500W of heat is applied to the heat dissipation surface of the evaporator based on the diamond micro-channel, the temperature of the lower surface is maintained to be 20 ℃, the temperature difference between the upper surface and the lower surface is theoretically simulated to be only 7 ℃, a good heat dissipation effect is displayed, and the heat dissipation requirement of a high-power electronic device can be met.
Example 2
And grinding the high-temperature molybdenum substrate with the composite transition layer for 15min by adopting diamond grinding paste with the particle size of 5 mu m, and washing for 2 times by adopting acetone. Placing the processed substrate into a high-energy activation plasma chamber to prepare a diamond film, wherein the distance between an anode and the substrate is 1.1cm, the deposition temperature is 950 ℃, the deposition pressure is 3.5Kpa, the cooling water temperature is less than or equal to 25 ℃, the Ar flow is 3.8SLM, H2Flow rate of 7SLM, CH4The initial growth flow is 120SCCM, and CH is added after each 100h of growth4The flow is adjusted up to 20SCCM, and CH is closed after 10min of re-nucleation4And keeping for 15 min. Then call back CH4To the growth flux. After 500h of growth, a diamond film having a thickness of 5mm was obtained. And grinding and polishing the obtained diamond thick film by using a grinding and polishing machine, wherein the thickness of the polished diamond thick film is 3.5 mm. The granularity of diamond abrasive is selected to be 400#, the rotating speed of the grinding disc is 50rmp, and the loading weight is 800 g. Structures of 25mm x 10mm size were cut on the diamond thick film using a laser cutter. The cutting parameters of the laser are as follows: the power was 120W, the sample feed rate was 150mm/min, and the number of cuts was 13. Construction of diamond particlesThe laser cutting power of the channel is 120W, the sample feeding speed is 80mm/min, the width of the micro-channel is 0.2mm, and the depth is 1.2 mm. Acid washing is used to remove surface impurities and graphite. The thermal conductivity of the obtained V-shaped section diamond micro-channel heat sink structure is 1630W/mK. The water medium is used as the heat transfer working medium, so that the heat dissipation effect is good, and the heat dissipation requirement of a high-power electronic device can be met.
Claims (6)
1. A preparation method of a diamond micro-channel heat sink for heat dissipation with ultrahigh heat flow density is characterized by comprising the following steps:
step 1: preparing an ultra-thick CVD diamond film;
1.1, selecting high-temperature molybdenum as a diamond thick film deposition substrate, and plating a composite transition layer on the surface of the molybdenum substrate in advance to reduce thermal stress concentration in the deposition process and improve the stripping yield;
1.2, placing the processed substrate into a high-energy activated plasma chamber to prepare a diamond film, setting an initial deposition process, increasing the methane concentration by 20-50sccm on the basis of growth flow at intervals of 50-100 hours, increasing high-energy carbon atom groups for a short time to bombard the surface to realize secondary nucleation, and adjusting the methane concentration back to the growth concentration after 10-25 min; then, hydrogen/argon plasma is used for etching for 5-10min to remove non-diamond carbon components possibly formed; the total deposition time is 300-600 h, and a diamond thick film with the thickness of 4-6mm is obtained;
step 2: grinding and polishing the diamond thick film;
polishing the obtained diamond thick film by using a grinding and polishing machine by adopting a mechanical grinding and polishing technology until the surface roughness is 0.5-3.2 mu m, so that the diamond thick film meets the requirement of the subsequent welding of a heat exchange surface of a microchannel, and simultaneously reduces the interface thermal resistance;
and step 3: forming the structure of the diamond thick film;
the diamond thick film has large internal stress, and the diamond thick film is easy to generate thermal stress concentration in the laser forming process to cause random cracking in the processing process; therefore, in the initial stage of forming, a low-power and low-speed laser cutting process laser is adopted, and a diamond special cutter is adopted, the laser wavelength is 1064nm, and a YAG laser generator is adopted;
and 4, step 4: constructing a microfluidic channel on the surface of the diamond film by laser cutting;
similarly, a micro-flow channel is constructed on the surface of the diamond thick film by using the laser micro-beam, and the size of a laser spot, the focusing depth, the light beam convergence angle, the cutting times and the cutting rate are accurately controlled; in order to obtain a specific micro-groove shape and depth-to-width ratio, the inclined height of the sample stage in the X-Y direction can be adjusted, or the opening angle of a laser beam can be adjusted in a small range;
the thickness of the diamond thick film material in a deposition state is more than or equal to 4mm, and the thickness of the micro-groove after processing is more than or equal to 3 mm.
2. The method for preparing the diamond micro-channel heat sink for ultra-high heat flow density heat dissipation according to claim 1, wherein the diamond thick film material adopts a high-temperature molybdenum material pre-plated with a composite transition layer as a substrate, and the composite transition layer is made of Ti, Mo, Si or W; the ultra-thick diamond film is prepared by adopting a direct current jet CVD method with an improved process.
3. The method for preparing the diamond micro-channel heat sink for ultra-high heat flow density heat dissipation according to claim 2, wherein the direct current jet CVD method of the improved process is as follows: intermittently adjusting the secondary nucleation process and assisting in H2the/Ar plasma processing technology realizes secondary re-nucleation, inhibits the abnormal growth of large columnar crystals, and improves the grain density of the diamond film, thereby ensuring that the effective growth thickness of the diamond thick film reaches more than 4 mm.
4. The method for preparing a diamond microchannel heat sink for ultra-high heat flow density heat dissipation according to claim 1, wherein the microchannel heat exchanger is made of full diamond material, and the thickness dimension of the microchannel is more than 3 mm.
5. The method for preparing the diamond microchannel heat sink for ultra-high heat flow density heat dissipation according to claim 1, wherein the microchannel heat exchanger adopts a special laser cutting machine for diamond to realize the shaping of diamond; and processing of different groove types is realized by adjusting the deflection angle of the X-Y axis of the laser and the opening angle of the laser.
6. The method for preparing a diamond microchannel heat sink for ultra-high heat flow density heat dissipation according to claim 1, wherein the heat exchanger with microgrooves controls the roughness of the thermal contact surface by mechanical grinding technology, so that the heat exchanger can meet the effects of minimum welding strength and thermal resistance, and the roughness is 0.5-3.2 μm.
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