CN112091208A - Heat-conducting copper powder with bimodal distribution characteristic and preparation method and application thereof - Google Patents
Heat-conducting copper powder with bimodal distribution characteristic and preparation method and application thereof Download PDFInfo
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 213
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 238000009826 distribution Methods 0.000 title claims abstract description 38
- 230000002902 bimodal effect Effects 0.000 title claims abstract description 37
- 238000005245 sintering Methods 0.000 claims abstract description 59
- 239000003979 granulating agent Substances 0.000 claims abstract description 53
- 238000002156 mixing Methods 0.000 claims abstract description 46
- 239000002245 particle Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000005469 granulation Methods 0.000 claims abstract description 7
- 230000003179 granulation Effects 0.000 claims abstract description 7
- 238000011068 loading method Methods 0.000 claims abstract description 3
- 238000007873 sieving Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 12
- 239000007788 liquid Substances 0.000 abstract description 12
- 230000017525 heat dissipation Effects 0.000 abstract description 4
- 239000007769 metal material Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 39
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 24
- 239000012752 auxiliary agent Substances 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 23
- 239000000203 mixture Substances 0.000 description 17
- 229910052802 copper Inorganic materials 0.000 description 16
- 239000010949 copper Substances 0.000 description 16
- 230000000694 effects Effects 0.000 description 16
- 238000012360 testing method Methods 0.000 description 16
- 238000012546 transfer Methods 0.000 description 16
- 229910021529 ammonia Inorganic materials 0.000 description 12
- 238000000354 decomposition reaction Methods 0.000 description 12
- 238000012856 packing Methods 0.000 description 11
- 238000013461 design Methods 0.000 description 7
- 239000004973 liquid crystal related substance Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 229910000570 Cupronickel Inorganic materials 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
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- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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Abstract
The invention belongs to the field of metal materials, and particularly relates to heat-conducting copper powder with a bimodal distribution characteristic, and a preparation method and application thereof. The method comprises the following steps: selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent for mixing granulation, and then sequentially carrying out loose loading sintering and crushing to obtain the heat-conducting copper powder with the characteristic of bimodal distribution. The invention can simply and efficiently prepare the heat-conducting copper powder with good heat-conducting property; the heat-conducting copper powder can be well used for preparing the liquid absorption core in the small-caliber sintered heat pipe; the prepared liquid absorption core has excellent heat conduction and heat dissipation performance.
Description
Technical Field
The invention belongs to the field of metal materials, and particularly relates to heat-conducting copper powder with a bimodal distribution characteristic, and a preparation method and application thereof.
Background
The Heat conduction pipe (Heat conduction tube) is used as a vapor-liquid phase change Heat transfer element, has the advantages of high Heat conductivity, good temperature uniformity, high reliability, no need of extra energy for driving and the like, is the highest efficiency in the Heat dissipation technical scheme, and can form a large-scale standardized thermal design scheme.
However, the heat transfer performance of the conventional heat pipe mainly depends on the wick structure inside the heat pipe, and the heat pipe is divided according to the type of wick, and can be divided into a groove type heat pipe, a sintered type heat pipe, and a composite type heat pipe. The sintered heat pipe is formed by sintering a heat-conducting copper powder, graphene or other materials to form a wick. With the light weight design and the light weight design of smart devices in recent years, the thickness of a tablet personal computer and a mobile phone can be reduced to about 5mm, a household television can be reduced to about 3mm even, so that the applicability of the traditional sintered copper tube is weakened, because the traditional sintered copper tube has a good phase change transmission effect for ensuring the whole heat conduction tube, a liquid absorption core needs to be ensured to have a certain thickness, but if the diameter of the sintered copper tube is reduced briefly, the inner diameter of the heat conduction tube is narrowed, and the gas phase transmission effect of the heat conduction tube is reduced, the traditional sintered copper tube is difficult to realize the light weight and light weight design, and is more difficult to be suitable for the existing smart devices with the light weight and light weight design.
In this regard, improvements in the wicking material of heat pipes have been made. Such as a graphene wick developed vigorously, which has very excellent heat transfer and thermal conductivity. However, graphene generally needs to be prepared by a vapor deposition method, such as anyhow, high-strength, malacopc, and the like, the chemical vapor deposition method of graphene prepares [ J ] a novel carbon material, 2011(01):71-80 ], plum chelate, wilting, anyui and wai, and the like, the copper-nickel alloy is used as a substrate for preparing graphene research [ J ] a functional material by the chemical vapor deposition method, 2012,43(023):3257-3260, and the like, the preparation method of the vapor deposition method disclosed in the documents is far more difficult than the conventional sintering preparation process, has a slightly lower yield, improves the cost of the sintering preparation process, and simultaneously is more expensive than copper, and the overall improvement of the heat conduction performance is realized, but the problems of cost improvement and preparation difficulty are also generated.
On the other hand, some researchers have also studied copper powder sintered heat pipes, such as Weibel J A, Kousalya A S, Fisher T S, et alured enhancement of boiling incipience in capillary-fed,ultra-thin sintered powder wicks[C]//IEEE Intersociety Conference on Thermal&IEEE,2012, the prepared sintered copper powder wick can bear the superheat degree of 437W/cm at 23 DEG C2The heat flux density of (2) is too high, so that the practical use effect is still limited, and the superheat degree is higher under the condition of simple copper material preparation, which indicates that the response capability is weaker under the condition of low pipe diameter, and the heat dissipation effect is difficult to generate in real time.
Disclosure of Invention
The invention provides heat-conducting copper powder with a bimodal distribution characteristic and a preparation method and application thereof, aiming at solving the problems that the traditional sintering heat pipe is difficult to realize light weight and light weight design, and partial sintering heat pipe is subjected to light weight and light weight design, or has performance problems of heat transfer performance reduction, superheat degree increase and the like, or has industrialization problems of cost increase, difficulty increase and the like.
The invention aims to:
firstly, preparing heat-conducting copper powder capable of replacing 99.5% of pure copper powder used by a traditional liquid absorption core through a simple process;
secondly, the heat conduction performance of the copper powder after the copper powder is sintered to form a liquid absorption core is improved;
and thirdly, ensuring that the superheat degree of the liquid absorption core formed after the heat-conducting copper powder is sintered is lower.
In order to achieve the purpose, the invention adopts the following technical scheme.
A preparation method of heat-conducting copper powder with bimodal distribution characteristics,
the method comprises the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent for mixing granulation, and then sequentially carrying out loose loading sintering and crushing to obtain the heat-conducting copper powder with the characteristic of bimodal distribution.
In the technical scheme of the invention, the copper powder with special bimodal distribution is prepared by mixing the copper powder with double particle sizes with a granulating agent, the overall preparation process is simple and efficient, porous copper powder can be obtained by simple mixing and granulating, and loose sintering and crushing, and tests show that the copper powder prepared by the process can greatly improve the limit heat flux density of a sintered heat pipe, remarkably reduce the superheat degree, improve the corresponding rate of the heat pipe and further improve the actual use effect.
In addition, the copper powder is high-purity copper powder which is used in the conventional process and meets the purity of 99.5 percent. The loose sintering is carried out in an ammonia decomposition heating furnace or a hydrogen furnace, and the sintering material formed after mixing and granulation is taken as a reference, an auxiliary agent with the total mass of 10-20 wt% of the sintering material is added, and the auxiliary agent is ethanol or cyclohexane, and the like. The technical effects of the additive amount of 10-20 wt% are relatively close, the additive amount is higher than 20 wt% and then waste of the additive is easily generated, the problem of agglomeration is easily caused, loose-packed sintering is not facilitated, and effective infiltration and auxiliary sintering cannot be formed due to too small amount of the additive.
As a preference, the first and second liquid crystal compositions are,
the mesh number of the crude copper powder is 60-200 meshes;
the mesh number of the fine copper powder is 500-1000 meshes.
Through tests, the heat-conducting copper powder prepared by matching the two copper powders in the mesh number range has a better using effect and higher comprehensive integrity and price ratio.
As a preference, the first and second liquid crystal compositions are,
the coarse copper powder and the fine copper powder are mixed according to the mass ratio of (3-5): (5-7) in the above ratio.
The mixing proportion can produce a better preparation effect, and the heat-conducting copper powder is ensured to have better performance.
As a preference, the first and second liquid crystal compositions are,
the granulating agent is PEG, PVB, PVA, Emultex FR728 or D60 solvent oil.
The granulating agent is easy to rapidly and thoroughly remove in the subsequent sintering process after use, the purity of the prepared heat-conducting copper powder is improved, and the purity can be ensured to reach more than 99.5%.
As a preference, the first and second liquid crystal compositions are,
the addition amount of the granulating agent is 0.5-2.0 wt% of the total mass of the coarse copper powder and the fine copper powder.
The addition amount can realize a good granulation effect, agglomeration is easily caused due to excessive addition amount, the particle size of powder obtained by mixing granulation is too large and uneven, the subsequent crushing difficulty is increased, or copper powder is separated again after loose-packed sintering, heat-conducting copper powder cannot be effectively prepared, and poor granulation effect is caused due to too small use amount.
As a preference, the first and second liquid crystal compositions are,
and after mixing and granulating, sieving by a 30-mesh sieve and drying.
The 30-mesh sieve can effectively screen out a small amount of powder with overlarge particle size formed by agglomeration, and tests show that the powder can generate relatively serious pulverization after loose sintering and cannot actually generate a good heat conduction effect.
As a preference, the first and second liquid crystal compositions are,
the loose sintering comprises the following steps: setting the sintering temperature to be 700-800 ℃ and the sintering time to be 45-75 min.
Sintering under the above temperature conditions and time conditions can achieve good sintering effects. Meanwhile, the loose sintering of the invention is carried out in an oxygen-free atmosphere.
A heat-conducting copper powder with bimodal distribution characteristics.
The characteristic peak distribution of the heat-conducting copper powder is shown in figure 1, and the diffraction peaks with the 2 theta values of 43 degrees, 50 degrees and 74 degrees are diffraction peaks of copper, wherein the diffraction peaks 1 with the angles of 43 degrees and 74 degrees are the same as the characteristic peak measured by fine copper powder, and the diffraction peak 2 with the angle of 50 degrees is the same as the characteristic peak measured by coarse copper powder. Therefore, the heat-conducting copper powder is obviously composed of fine copper powder and coarse copper powder, and the microscopic characteristics of the original fine copper powder and the original coarse copper powder are reserved.
Application of heat-conducting copper powder in preparation of heat-conducting pipe liquid absorption cores.
The copper powder has very excellent thermal conductivity, can replace the traditional 99.5 percent pure copper powder when being used for preparing the heat-conducting pipe liquid absorption core, effectively improves the ultimate heat transfer power of the heat pipe, reduces the superheat degree, improves the performance of the heat-conducting pipe, and can realize good effect under the condition of smaller thickness.
The invention has the beneficial effects that:
1) the heat-conducting copper powder with good heat-conducting property can be simply and efficiently prepared;
2) the heat-conducting copper powder can be well used for preparing the liquid absorption core in the small-caliber sintered heat pipe;
3) the prepared liquid absorption core has excellent heat conduction and heat dissipation performance.
Drawings
FIG. 1 is an XRD pattern of copper powder prepared in example 1 of the present invention.
Detailed Description
The invention is described in further detail below with reference to specific embodiments and the attached drawing figures. Those skilled in the art will be able to implement the invention based on these teachings. Moreover, the embodiments of the present invention described in the following description are generally only some embodiments of the present invention, and not all embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Unless otherwise specified, the raw materials used in the examples of the present invention are all commercially available or available to those skilled in the art; unless otherwise specified, the methods used in the examples of the present invention are all those known to those skilled in the art.
Unless otherwise stated, the measured superheat degree in the embodiment of the invention refers to the lowest temperature difference from the evaporation state to the boiling state, and the measurement of the limit heat transfer power in the application refers to the limit heat transfer power in the state of 120 ℃.
Example 1
A heat-conducting copper powder with a bimodal distribution characteristic has an XRD diffraction pattern shown in figure 1, and has characteristic peaks with 2 theta values of 43 degrees, 50 degrees and 74 degrees, wherein the 43 degrees and 74 degrees are characteristic peaks of fine copper powder, and the 50.42 degrees are characteristic peaks of coarse copper powder;
the preparation method comprises the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent, mixing, granulating, sieving by a 30-mesh sieve, drying, taking ethanol as an auxiliary agent, and mixing the auxiliary agent and a sintering material according to a mass ratio of 15: 100, placing the mixture in an ammonia decomposition furnace, loosely packing, sintering, crushing, and sieving by a 100-mesh sieve to obtain the heat-conducting copper powder with the characteristic of bimodal distribution. The specific preparation materials and parameters are shown in the following table 1.
Table 1: materials and preparation parameters used in example 1
In the table: the addition amount of the granulating agent is the proportion of the mass of the granulating agent to the total mass of the coarse copper powder and the fine copper powder.
Example 2
A heat-conducting copper powder with a bimodal distribution characteristic has an XRD diffraction pattern similar to that of example 1 and has characteristic peaks with 2 theta values of 43 degrees, 50 degrees and 74 degrees, wherein the 43 degrees and 74 degrees are characteristic peaks of fine copper powder, and the 50 degrees is characteristic peak of coarse copper powder;
the preparation method comprises the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent, mixing, granulating, sieving by a 30-mesh sieve, drying, taking ethanol as an auxiliary agent, and mixing the auxiliary agent and a sintering material according to a mass ratio of 15: 100, placing the mixture in an ammonia decomposition furnace, loosely packing, sintering, crushing, and sieving by a 100-mesh sieve to obtain the heat-conducting copper powder with the characteristic of bimodal distribution. The specific preparation materials and parameters are shown in the following table 2.
Table 2: materials and preparation parameters used in example 2
In the table: the addition amount of the granulating agent is the proportion of the mass of the granulating agent to the total mass of the coarse copper powder and the fine copper powder.
Example 3
A heat-conducting copper powder with a bimodal distribution characteristic has an XRD diffraction pattern similar to that of example 1 and has characteristic peaks with 2 theta values of 43 degrees, 50 degrees and 74 degrees, wherein the 43 degrees and 74 degrees are characteristic peaks of fine copper powder, and the 50 degrees is characteristic peak of coarse copper powder;
the preparation method comprises the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent, mixing, granulating, sieving by a 30-mesh sieve, drying, taking ethanol as an auxiliary agent, and mixing the auxiliary agent and a sintering material according to a mass ratio of 15: 100, placing the mixture in an ammonia decomposition furnace, loosely packing, sintering, crushing, and sieving by a 100-mesh sieve to obtain the heat-conducting copper powder with the characteristic of bimodal distribution. The specific preparation materials and parameters are shown in Table 3 below.
Table 3: materials and preparation parameters used in example 3
In the table: the addition amount of the granulating agent is the proportion of the mass of the granulating agent to the total mass of the coarse copper powder and the fine copper powder.
Example 4
A heat-conducting copper powder with a bimodal distribution characteristic has an XRD diffraction pattern similar to that of example 1 and has characteristic peaks with 2 theta values of 43 degrees, 50 degrees and 74 degrees, wherein the 43 degrees and 74 degrees are characteristic peaks of fine copper powder, and the 50 degrees is characteristic peak of coarse copper powder;
the preparation method comprises the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent, mixing, granulating, sieving by a 30-mesh sieve, drying, taking ethanol as an auxiliary agent, and mixing the auxiliary agent and a sintering material according to a mass ratio of 15: 100, placing the mixture in an ammonia decomposition furnace, loosely packing, sintering, crushing, and sieving by a 100-mesh sieve to obtain the heat-conducting copper powder with the characteristic of bimodal distribution. The specific preparation materials and parameters are shown in Table 4 below.
Table 4: materials and preparation parameters used in example 4
In the table: the addition amount of the granulating agent is the proportion of the mass of the granulating agent to the total mass of the coarse copper powder and the fine copper powder.
Example 5
A heat-conducting copper powder with a bimodal distribution characteristic has an XRD diffraction pattern similar to that of example 1 and has characteristic peaks with 2 theta values of 43 degrees, 50 degrees and 74 degrees, wherein the 43 degrees and 74 degrees are characteristic peaks of fine copper powder, and the 50 degrees is characteristic peak of coarse copper powder;
the preparation method comprises the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent, mixing, granulating, sieving by a 30-mesh sieve, drying, taking ethanol as an auxiliary agent, and mixing the auxiliary agent and a sintering material according to a mass ratio of 15: 100, placing the mixture in an ammonia decomposition furnace, loosely packing, sintering, crushing, and sieving by a 100-mesh sieve to obtain the heat-conducting copper powder with the characteristic of bimodal distribution. The specific preparation materials and parameters are shown in Table 5 below.
Table 5: materials and preparation parameters used in example 5
In the table: the addition amount of the granulating agent is the proportion of the mass of the granulating agent to the total mass of the coarse copper powder and the fine copper powder.
Example 6
A heat-conducting copper powder with a bimodal distribution characteristic has an XRD diffraction pattern similar to that of example 1 and has characteristic peaks with 2 theta values of 43 degrees, 50 degrees and 74 degrees, wherein the 43 degrees and 74 degrees are characteristic peaks of fine copper powder, and the 50 degrees is characteristic peak of coarse copper powder;
the preparation method comprises the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent, mixing, granulating, sieving by a 30-mesh sieve, drying, taking ethanol as an auxiliary agent, and mixing the auxiliary agent and a sintering material according to a mass ratio of 15: 100, placing the mixture in an ammonia decomposition furnace, loosely packing, sintering, crushing, and sieving by a 100-mesh sieve to obtain the heat-conducting copper powder with the characteristic of bimodal distribution. The specific preparation materials and parameters are shown in Table 6 below.
Table 6: materials and preparation parameters used in example 6
In the table: the addition amount of the granulating agent is the proportion of the mass of the granulating agent to the total mass of the coarse copper powder and the fine copper powder.
Comparative example 1
A heat-conducting copper powder is prepared by the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent, mixing, granulating, sieving by a 30-mesh sieve, drying, taking ethanol as an auxiliary agent, and mixing the auxiliary agent and a sintering material according to a mass ratio of 15: 100, placing the mixture in an ammonia decomposition furnace, loosely packing, sintering, crushing, and sieving by a 100-mesh sieve to obtain the heat-conducting copper powder with the characteristic of bimodal distribution. The specific preparation materials and parameters are shown in Table 7 below.
Table 7: materials and preparation parameters used in comparative example 1
In the table: the addition amount of the granulating agent is the proportion of the mass of the granulating agent to the total mass of the coarse copper powder and the fine copper powder.
Comparative example 2
A heat-conducting copper powder is prepared by the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent, mixing, granulating, sieving by a 30-mesh sieve, drying, taking ethanol as an auxiliary agent, and mixing the auxiliary agent and a sintering material according to a mass ratio of 15: 100, placing the mixture in an ammonia decomposition furnace, loosely packing, sintering, crushing, and sieving by a 100-mesh sieve to obtain the heat-conducting copper powder with the characteristic of bimodal distribution. The specific preparation materials and parameters are shown in Table 8 below.
Table 8: materials and preparation parameters used in comparative example 2
In the table: the addition amount of the granulating agent is the proportion of the mass of the granulating agent to the total mass of the coarse copper powder and the fine copper powder.
Comparative example 3
A heat-conducting copper powder is prepared by the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent, mixing, granulating, sieving by a 30-mesh sieve, drying, taking ethanol as an auxiliary agent, and mixing the auxiliary agent and a sintering material according to a mass ratio of 15: 100, placing the mixture in an ammonia decomposition furnace, loosely packing, sintering, crushing, and sieving by a 100-mesh sieve to obtain the heat-conducting copper powder with the characteristic of bimodal distribution. The specific preparation materials and parameters are shown in Table 9 below.
Table 9: materials and preparation parameters used in comparative example 3
In the table: the addition amount of the granulating agent is the proportion of the mass of the granulating agent to the total mass of the coarse copper powder and the fine copper powder.
Comparative example 4
A heat-conducting copper powder is prepared by the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent, mixing, granulating, sieving by a 30-mesh sieve, drying, taking ethanol as an auxiliary agent, and mixing the auxiliary agent and a sintering material according to a mass ratio of 15: 100, placing the mixture in an ammonia decomposition furnace, loosely packing, sintering, crushing, and sieving by a 100-mesh sieve to obtain the heat-conducting copper powder with the characteristic of bimodal distribution. The specific preparation materials and parameters are shown in Table 10 below.
Table 10: materials and preparation parameters used in comparative example 4
In the table: the addition amount of the granulating agent is the proportion of the mass of the granulating agent to the total mass of the coarse copper powder and the fine copper powder.
Comparative example 5
A heat-conducting copper powder is prepared by the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent, mixing, granulating, sieving by a 10-mesh sieve, drying, taking ethanol as an auxiliary agent, and mixing the auxiliary agent and a sintering material according to a mass ratio of 15: 100, placing the mixture in an ammonia decomposition furnace, loosely packing, sintering, crushing, and sieving by a 100-mesh sieve to obtain the heat-conducting copper powder with the characteristic of bimodal distribution. The specific preparation materials and parameters are shown in Table 11 below.
Table 11: materials and preparation parameters used in comparative example 5
In the table: the addition amount of the granulating agent is the proportion of the mass of the granulating agent to the total mass of the coarse copper powder and the fine copper powder.
Testing
Application tests were conducted on the heat-conductive copper powders obtained in examples 1 to 6 and comparative examples 1 to 5.
The prepared heat-conducting copper powder is made into a liquid absorption core on the inner wall of a heat-conducting pipe according to the following conventional process: firstly, putting a red copper pipe with the outer diameter of 1.8mm and the inner diameter of 1.2mm into dilute sulfuric acid by using a tool for ultrasonic cleaning, coaxially inserting a straight thin rod steel rod with the outer diameter of 0.8mm into the red copper pipe after cleaning, sealing the bottom of the copper pipe by using a copper sheet, filling heat-conducting copper powder between the straight thin rod steel rod and the red copper pipe, placing the copper pipe in a nitrogen atmosphere for sintering at 850 ℃ for 60min after filling, and then drawing out the straight thin rod steel rod to obtain the heat-conducting pipe.
The test items include a superheat degree test and a limit heat transfer power test.
The test results are shown in table 12 below.
Table 12: test results
| Source of heat conductive copper powder | Limiting heat transfer power/W.cm-2 | Degree of superheat/. degree.C |
| Example 1 | 473 | 11.4 |
| Example 2 | 468 | 11.8 |
| Example 3 | 474 | 11.2 |
| Example 4 | 466 | 12.6 |
| Example 5 | 472 | 11.4 |
| Example 6 | 473 | 11.6 |
| Comparative example 1 | 442 | 15.1 |
| Comparative example 2 | 483 | 12.2 |
| Comparative example 3 | 419 | 18.7 |
| Comparative example 4 | 406 | 23.4 |
| Comparative example 5 | 422 | 16.9 |
As is evident from the test results in the above table, the ultimate heat transfer power of the heat pipes made of the heat-conducting copper powder in examples 1-6 is substantially maintained at 460W/cm2Above, the superheat degree can be basically kept below 13 ℃, which shows that the heat-conducting and heat-dissipating device has good heat-dissipating performance and good heat-dissipating response capability. The description will be made one by one based on example 1.
Example 2 increased the particle size of the copper powder used compared to example 1, with a slight deterioration in both ultimate heat transfer capacity and superheat, but was essentially equivalent and still at a higher level, as in example 3 with a small but still insignificant optimization of the performance after reduction of the particle size of the copper powder. It is shown that the mesh number of the copper powder used is selected within the range defined in the present invention, and the influence on the thermal conductivity is not significant. However, in this case, comparing the data measured in comparative example 5, the copper powder used in comparative example 5 has a particle size significantly larger than the range defined in the present invention, resulting in a significant deterioration in its performance, and shows no bimodal distribution characteristic in its XRD characterization pattern, which has only a single characteristic peak with a 2 θ value of about 50 °.
Example 4 the amount ratio of the crude copper powder was increased as compared with example 1, resulting in a significant decrease in the performance thereof, and the specific surface area test showed a significant decrease in the specific surface area as compared with example 1, which was considered by researchers to be the main cause of the decrease in the performance thereof. In the same way, comparative example 1 added more coarse copper powder than example 4, resulting in a further reduction in its properties. Compared with the embodiment 1, the comparative example 2 is added with more fine copper powder, the limit heat transfer power is obviously improved, the degree of superheat generates a small amount of deterioration, but in fact, the cost is also improved compared with the embodiment 1, the cost performance is slightly lower than that of the embodiment 1, and the most important point is that the whole compactness of the liquid absorption core is improved due to the adoption of the excessive fine copper powder, and the liquid phase boiling is not facilitated.
Compared with the embodiment 1, the embodiment 5 and the embodiment 6 respectively reduce and improve the dosage of the granulating agent within the protection range defined by the invention, and the influence on the limit heat transfer power and the superheat degree is basically negligible. In contrast, in comparative example 3, too little granulating agent is used, so that the actual fine copper powder and coarse copper powder are less compounded, and in an XRD characterization test, a test result shows that although a characteristic peak with a 2 theta value of 50 degrees and characteristic peaks with 2 theta values of 43 degrees and 74 degrees are generated in most cases, the ratio of the two is continuously fluctuated. And in the comparative example 4, the dosage of the granulating agent is too large, the too large dosage of the granulating agent easily causes too much granulating agent to exist between the fine copper powder and the crude copper powder, and the too much granulating agent causes poor sintering effect, so that the product performance is influenced, and even the performance is worse than that of the comparative example 3.
Example 7
The same procedure as in example 1 was followed and the same heat pipes as above were prepared and tested, except that:
the types of granulating agents were varied, and the specific types of granulating agents used are shown in table 13 below.
Table 13: types of granulating agents used in example 7 and corresponding test results
As can be seen from the table above, the influence of the selection of the granulating agent on the actual heat-conducting copper powder is not large, and research and development personnel can realize similar technical effects when judging that the conventional granulating agent for copper processing can be used.
Example 8
The same procedure as in example 1 was followed and the same heat pipes as above were prepared and tested, except that:
the loose sintering temperature and time were varied as shown in table 14 below.
Table 14: example 8 loose-pack sintering conditions and corresponding test results
| Sintering temperature/. degree.C | Sintering time/min | Limiting heat transfer power/W.cm-2 | Degree of superheat/. degree.C |
| 700 | 60 | 471 | 11.6 |
| 700 | 75 | 472 | 11.6 |
| 800 | 60 | 473 | 11.3 |
| 800 | 45 | 474 | 11.5 |
| 650 | 60 | 459 | 12.3 |
| 850 | 60 | 422 | 16.7 |
As can be seen from the above table, the influence on the limit heat transfer power and the degree of superheat is small within the sintering parameter range defined by the present invention. However, when sintering is carried out at a lower temperature, the sintering effect is poor, and both properties are weakened to some extent. And excessive sintering is easy to generate when sintering is carried out under the condition of higher temperature, research and development personnel find that a great amount of caking is generated in the sintering process, so that the microstructure of the heat-conducting copper powder is actually damaged after subsequent crushing, and the two performances of the limit heat transfer power and the superheat degree of the heat-conducting copper powder are remarkably reduced.
Claims (9)
1. A preparation method of heat-conducting copper powder with bimodal distribution characteristics is characterized in that,
the method comprises the following steps:
selecting coarse copper powder with larger particle size and fine copper powder with smaller particle size respectively, mixing the coarse copper powder and the fine copper powder, adding a granulating agent for mixing granulation, and then sequentially carrying out loose loading sintering and crushing to obtain the heat-conducting copper powder with the characteristic of bimodal distribution.
2. The method for preparing the heat-conducting copper powder with the characteristic of bimodal distribution according to claim 1,
the mesh number of the crude copper powder is 60-200 meshes;
the mesh number of the fine copper powder is 500-1000 meshes.
3. The method for preparing the heat-conducting copper powder with the characteristic of bimodal distribution as claimed in claim 1 or 2,
the coarse copper powder and the fine copper powder are mixed according to the mass ratio of (3-5): (5-7) in the above ratio.
4. The method for preparing the heat-conducting copper powder with the characteristic of bimodal distribution according to claim 1,
the granulating agent is PEG, PVB, PVA, Emultex FR728 or D60 solvent oil.
5. The method for preparing the heat-conducting copper powder with the characteristic of bimodal distribution as claimed in claim 1 or 4,
the addition amount of the granulating agent is 0.5-2.0 wt% of the total mass of the coarse copper powder and the fine copper powder.
6. The method for preparing the heat-conducting copper powder with the characteristic of bimodal distribution according to claim 1,
and after mixing and granulating, sieving by a 30-mesh sieve and drying.
7. The method for preparing the heat-conducting copper powder with the characteristic of bimodal distribution according to claim 1,
the loose sintering comprises the following steps: setting the sintering temperature to be 700-800 ℃ and the sintering time to be 45-75 min.
8. A thermally conductive copper powder characterized by a bimodal distribution produced by the method of claim 1 or 2 or 3 or 4 or 5 or 6 or 7.
9. Use of thermally conductive copper powder according to claim 8 for the preparation of a heat-pipe wick.
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