CN116179924A - Particle reinforced high specific heat transfer alloy and preparation method thereof - Google Patents
Particle reinforced high specific heat transfer alloy and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/04—Alloys containing less than 50% by weight of each constituent containing tin or lead
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0005—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with at least one oxide and at least one of carbides, nitrides, borides or silicides as the main non-metallic constituents
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- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0042—Matrix based on low melting metals, Pb, Sn, In, Zn, Cd or alloys thereof
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- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/62—Quenching devices
- C21D1/63—Quenching devices for bath quenching
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/02—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for springs
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Abstract
The invention discloses a particle reinforced high specific heat transfer alloy and a preparation method thereof. The particle reinforced high specific heat transfer alloy takes eutectic alloy composed of Sn, bi and Zn low-melting point metal elements as matrix alloy, and nano particles as reinforcing phase to regulate the specific heat capacity of the alloy. The composite heat transfer alloy obtained by the invention has the advantages of high heat conductivity, high specific heat capacity, high heat stability, no safety risk and the like; the particle reinforced high specific heat transfer alloy is used as a heat transfer medium, so that the weakness of low specific heat capacity of an alloy material can be pertinently improved, more heat is conducted, the volume of a cooling device is greatly reduced, and the utilization rate of a quenching tank is improved; the composite heat transfer alloy prepared by the invention overcomes the defects of the existing quenching liquid cooling medium, and has wide application prospect along with the development of the intelligent manufacturing level of the leaf spring industry.
Description
Technical Field
The invention relates to the technical field of quenching cooling liquid for heat treatment of automobile leaf springs, in particular to a particle reinforced high specific heat transfer alloy and a preparation method thereof.
Background
Along with the continuous promotion of automation, intelligent level of automobile leaf spring manufacturing trade, leaf spring production line's efficiency is higher and higher, and leaf spring heat treatment in-process, especially when the hierarchical quenching, the temperature of quenching liquid rises too fast, very big influence the quenching quality of leaf spring, select high efficiency, wide temperature range's heat transfer medium to be used to be crucial to the production efficiency and the stable quality of leaf spring product.
In the selection of different cooling media, water or heat conduction oil is generally used for cooling the heat treatment quenching liquid, but the defects of pipeline pressure rising, huge volume of a heat exchange device and the like caused by low heat transfer efficiency and easy evaporation of water are often required to reduce production efficiency to meet heat dissipation requirements, and the heat conduction oil has insufficient heat stability, is easy to deteriorate in the long-term use process and has higher production cost.
In order to meet the production requirements of large-scale and high-efficiency production, a new ideal cooling medium with the characteristics of high heat transfer efficiency, high thermal stability, small pipeline corrosiveness and the like needs to be searched.
Disclosure of Invention
The invention aims to overcome the technical defects, and provides a particle reinforced high specific heat transfer alloy and a preparation method thereof, which solve the technical problems that the traditional cooling medium in the prior art cannot achieve low cost, high heat transfer efficiency, high heat stability and low pipeline corrosiveness.
In a first aspect, the invention provides a particle-reinforced high specific heat transfer alloy, which uses eutectic alloy composed of Sn, bi and Zn low-melting-point metal elements as a matrix alloy and nano particles as a reinforcing phase to regulate the specific heat capacity of the alloy.
In a second aspect, the present invention provides a method for preparing a particle-reinforced high specific heat transfer alloy, comprising the steps of:
mixing and smelting Sn ingots, bi ingots and Zn grains, and cooling to obtain a matrix alloy;
and (3) preparing the matrix alloy into powder, then adding nano particles and water-soluble auxiliary agents, uniformly mixing, remelting and mixing, and cooling to obtain the particle-reinforced high-specific heat transfer alloy.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the low-melting-point ternary eutectic alloy is adopted as a matrix, and the defect of low specific heat capacity of an alloy material is improved by adding nano particles in a targeted manner, so that the obtained composite heat transfer alloy has the advantages of high heat conductivity, high specific heat capacity, high heat stability, no safety risk and the like; the particle reinforced high specific heat transfer alloy is used as a heat transfer medium, so that the weakness of low specific heat capacity of an alloy material can be pertinently improved, more heat is conducted, the volume of a cooling device is greatly reduced, and the utilization rate of a quenching tank is improved; the composite heat transfer alloy prepared by the invention overcomes the defects of the existing quenching liquid cooling medium, and has wide application prospect along with the development of the intelligent manufacturing level of the leaf spring industry.
Drawings
FIG. 1 is a microscopic morphology image of the particle enhanced high specific heat transfer alloy of example 1;
FIG. 2 is an XRD pattern for the particle enhanced high specific heat transfer alloy of example 1;
FIG. 3 is a DSC plot of the particle reinforced high specific heat transfer alloy of example 1;
FIG. 4 is a thermal conductivity profile of the particle reinforced high specific heat transfer alloy of example 1;
FIG. 5 is a microscopic morphology image of the particle enhanced high specific heat transfer alloy of example 2;
FIG. 6 is an XRD pattern for the particle enhanced high specific heat transfer alloy of example 2;
FIG. 7 is a DSC plot of the particle reinforced high specific heat transfer alloy of example 2;
FIG. 8 is a thermal conductivity map of the particle reinforced high specific heat transfer alloy of example 2;
FIG. 9 is a microscopic morphology image of the particle enhanced high specific heat transfer alloy of example 3;
FIG. 10 is an XRD pattern for the particle enhanced high specific heat transfer alloy of example 3;
FIG. 11 is a DSC plot of the particle reinforced high specific heat transfer alloy of example 3;
fig. 12 is a thermal conductivity profile of the particle reinforced high specific heat transfer alloy of example 3.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In a first aspect, the invention provides a particle-reinforced high specific heat transfer alloy, which uses eutectic alloy composed of Sn, bi and Zn low-melting-point metal elements as a matrix alloy and nano particles as a reinforcing phase to regulate the specific heat capacity of the alloy.
In this embodiment, the matrix alloy has a mass fraction of Sn of 46 to 48wt.%, a mass fraction of Bi of 49 to 52wt.%, and a mass fraction of Zn of 1 to 3wt.%.
In this embodiment, the nanoparticle is at least one of a samarium oxide nanoparticle, a tungsten carbide nanoparticle, and a nickel nanoparticle. Further, the mass fraction of the nanoparticles is 0.4-1wt.% of the high specific heat transfer alloy. If the addition amount of the nano particles is too low, the effect cannot be achieved, and if the addition amount of the nano particles is too high, the agglomeration effect of the nano particles can occur, the particle size is obviously increased, and the enhancement effect is reduced. Within this content range, the resulting particle-reinforced high specific heat transfer alloy has optimal properties.
In this embodiment, the purity of the alloy material is 99.9% or more, and the average particle size of the nanoparticles is 30 to 60nm, and more preferably 40nm.
The specific heat capacity of the particle reinforced high specific heat transfer alloy is improved by more than 2 times compared with that of a matrix alloy, and the heat conductivity coefficient is 47 W.m -1 ·K -1 The above.
In a second aspect, the present invention provides a method for preparing a particle-reinforced high specific heat transfer alloy, comprising the steps of:
s1, mixing and smelting Sn ingots, bi ingots and Zn grains, and cooling to obtain a matrix alloy;
s2, preparing the matrix alloy into powder, then adding nano particles and water-soluble auxiliary agents, uniformly mixing, remelting and mixing, and cooling to obtain the particle-reinforced high-specific heat transfer alloy.
In this embodiment, the smelting tool is baked prior to smelting. The method comprises the following steps: heating the smelting furnace to 300 ℃, putting the graphite crucible and the metal mold into the smelting furnace, and preserving heat for 10-20 min. In order to prevent alloy solution from adhering to the inner wall of the crucible and affecting the components and performance of the alloy due to impurities in the crucible and the mold, a layer of release agent is coated on the inner wall of the crucible before the graphite crucible is put into a pit furnace for preheating, and meanwhile, the release agent is coated on the inner wall of the mold, so that the alloy sample is conveniently taken out.
In this embodiment, the smelting process includes: adding the weighed Sn ingot into a lead-free tin furnace, heating to 250-270 ℃, preserving heat for 20-40 minutes, adding the weighed Bi ingot after the Sn ingot is melted, adjusting the heating temperature to 400-450 ℃ after the Bi ingot is melted, adding Zn particles, preserving heat until the Bi particles are completely melted, adjusting the heating temperature to 400-420 ℃, and standing and preserving heat for 20-40 minutes. In the process, a tool is required to stir the alloy melt uniformly, and in order to prevent the alloy from reacting with air in the melting process, active carbon powder is covered on the surface of the liquid metal, and after the liquid alloy is mixed uniformly, a skimming ladle is used for cleaning the active carbon powder covered on the surface of the liquid metal in the crucible.
In the embodiment, after the smelting process is finished, molten metal is rapidly poured into a die, and after the molten metal is naturally cooled to room temperature, an alloy ingot is taken out to obtain a matrix alloy.
In this embodiment, the base alloy is made into powder by a ball mill.
In the embodiment, the water-soluble auxiliary agent is a composite organic liquid material with the capacity of breaking oxidation of the metal surface, wherein succinic acid accounts for 1.5-2 wt%, adipic acid accounts for 1.0-1.5 wt%, salicylic acid accounts for 0.5-1 wt%, and the balance is ethanol. Further, the mass fraction of the water-soluble auxiliary agent is 18-20wt.% of the composite alloy powder (matrix alloy+nanoparticles).
In this embodiment, the temperature of the remelting is 140 to 160 ℃, the heat preservation time is 10 to 20 minutes, and the remelting is performed in an inert atmosphere (such as nitrogen, argon, etc.). If the remelting temperature is too low, the alloy cannot be melted, and the effect of uniform components cannot be achieved; if the remelting temperature is too high, alloying of nano Ni particles can be possibly caused, the proportion of Ni existing in the form of simple substance second phase particles is reduced, and the strengthening effect is affected. In addition, the excessively high temperature has adverse effects on energy consumption, personnel labor, production cost and the like. Meanwhile, in the process, in order to reduce the oxidation of the alloy, a smelting furnace cover is required to be covered in the smelting process, and argon protective atmosphere is added.
In this embodiment, the number of remelting is 2 to 3. Cooling to room temperature after the remelting is finished, and casting after remelting is finished once again after complete solidification, so that the components of the material are ensured to be uniform.
Examples 1 to 3
Examples 1-3 provide a method for preparing a particle-reinforced high specific heat transfer alloy comprising the steps of:
(1) All smelting tools must be dried prior to smelting. Firstly, heating a smelting furnace to 300 ℃, putting a graphite crucible and a metal mold into the smelting furnace, and preserving heat for 10min. In order to prevent alloy solution from adhering to the inner wall of the crucible and affecting the components and performance of the alloy due to impurities in the crucible and the mold, a layer of release agent is coated on the inner wall of the crucible before the graphite crucible is put into a pit furnace for preheating, and meanwhile, the release agent is coated on the inner wall of the mold, so that the alloy sample is conveniently taken out.
(2) According to the proportion shown in Table 1, the weighed Sn ingot is added into a lead-free tin furnace, heated to 250-270 ℃ for melting, and kept for 30 minutes. Adding the weighed Bi ingot after the Sn ingot is melted, adjusting the heating temperature to 400-450 ℃ after the Bi ingot is melted, adding Zn particles, and preserving the temperature until the Bi particles are completely melted. The alloy melt is stirred uniformly by a tool, and the surface of the liquid metal is covered by activated carbon powder in order to prevent the alloy from reacting with air in the melting process. Heating temperature is regulated to 400-420 ℃, and standing and heat preservation are carried out for 30 minutes.
(3) After the liquid alloy is uniformly mixed, the active carbon powder covered on the surface of the liquid metal in the crucible is cleaned by a skimming ladle. And then pouring the molten metal into a cylindrical metal mold rapidly, and taking out the alloy cast ingot after the molten metal is naturally cooled to room temperature, thus completing the preparation of the matrix alloy.
(4) The method comprises the steps of preparing matrix alloy into powder by using a ball mill, mixing matrix alloy powder and nano particles according to the proportion of table 1, adding a water-soluble cosolvent (succinic acid accounts for 1.5 wt%, adipic acid accounts for 1.2 wt%, salicylic acid accounts for 0.7 wt%, and the balance is ethanol) accounting for 18 wt% of the total mass of the composite alloy powder, stirring pasty composite powder for 30min to fully mix, then placing the composite alloy powder into a vacuum melting furnace with the set temperature of 150 ℃ for remelting and mixing, covering a melting furnace cover in the melting process for reducing the oxidation of the alloy, adding argon protective atmosphere, cooling to room temperature after preserving heat for ten minutes, remelting once again after complete solidification, and casting to ensure the uniformity of the components of the material.
TABLE 1 alloy composition design values for particle-reinforced high specific heat transfer alloys obtained in examples 1 to 3
(in Table 1, the sum of the compositions of the matrix alloy was 99.5%, and the nanoparticles were 0.5% of the total mass of the composite alloy powder (matrix alloy+nanoparticles))
Table 2 alloy composition measurements of the particle-reinforced high specific heat transfer alloys obtained in examples 1 to 3
(the sum of the compositions of the particle-reinforced high specific heat transfer alloys is 100% in Table 2).
Referring to FIGS. 1-12, the particle-reinforced high specific heat transfer alloy prepared according to the present invention has Cp at 12Jg -1 K -1 The thermal conductivity is 47 W.m -1 ·K -1 The above.
Compared with the prior art, the invention has the beneficial effects that:
(1) The particle-reinforced high-specific heat transfer alloy takes the ternary eutectic alloy as a matrix, nano particles are added to regulate the specific heat capacity of the alloy, so that the heat exchange efficiency of a heat transfer medium is greatly improved, and the energy cost is saved.
(2) Compared with water or heat conducting oil, liquid metal and other heat transfer media, the particle reinforced high-specific heat transfer alloy has the characteristics of high specific heat capacity and high heat transfer efficiency, and because the density and the heat conductivity of the particle reinforced high-specific heat transfer alloy are high, the cooling medium in unit volume can conduct more heat, the volume of the cooling device is greatly reduced, and the utilization rate of a quenching tank is improved.
(3) The particle reinforced high specific heat transfer alloy adopts the powder metallurgy and secondary forming modes, nano particles are added into the matrix alloy to form an independent second heat conduction phase, the raw materials are low in price, the operation method is simple, the alloying degree is high in the preparation process, the metal oxidation is less, and the heat transfer effect per unit volume is better.
(4) The particle reinforced high-specific heat transfer alloy has good high-temperature stability, can be used for a long time, does not deteriorate, has small volume change before and after phase change, is not easy to cause pipeline leakage, and is safe and risk-free.
(5) The invention has simple process, convenient operation and low cost, does not need to modify the existing production line equipment, can effectively improve the heat treatment efficiency of a large number of plate springs and improves the economic benefit of enterprises.
The above-described embodiments of the present invention do not limit the scope of the present invention. Any other corresponding changes and modifications made in accordance with the technical idea of the present invention shall be included in the scope of the claims of the present invention.
Claims (10)
1. The particle reinforced high specific heat transfer alloy is characterized in that the particle reinforced high specific heat transfer alloy takes eutectic alloy composed of Sn, bi and Zn low-melting-point metal elements as a matrix alloy, and nano particles as a reinforcing phase to regulate the specific heat capacity of the alloy.
2. The particle reinforced high specific heat transfer alloy of claim 1, wherein the matrix alloy has a mass fraction of Sn of 46-48wt.%, a mass fraction of Bi of 49-52wt.%, and a mass fraction of Zn of 1-3wt.%.
3. The particle reinforced high specific heat transfer alloy of claim 1, wherein the nanoparticles are at least one of nano samarium oxide particles, nano tungsten carbide particles, nano nickel particles.
4. The particle reinforced high specific heat transfer alloy of claim 1, wherein the mass fraction of the nanoparticles is 0.4-1wt.% of the total mass of the high specific heat transfer alloy.
5. The particle-reinforced high specific heat transfer alloy of claim 1, wherein the purity of the alloy feedstock is 99.9% or more and the average particle size of the nanoparticles is 30 to 60nm.
6. A method of preparing a particle reinforced high specific heat transfer alloy as claimed in any one of claims 1 to 5 comprising the steps of:
mixing and smelting Sn ingots, bi ingots and Zn grains, and cooling to obtain a matrix alloy;
and (3) preparing the matrix alloy into powder, then adding nano particles and water-soluble auxiliary agents, uniformly mixing, remelting and mixing, and cooling to obtain the particle-reinforced high-specific heat transfer alloy.
7. The method of producing a particle-reinforced high specific heat transfer alloy as claimed in claim 6, wherein the smelting process comprises: adding the weighed Sn ingot into a lead-free tin furnace, heating to 250-270 ℃, preserving heat for 20-40 minutes, adding the weighed Bi ingot after the Sn ingot is melted, adjusting the heating temperature to 400-450 ℃ after the Bi ingot is melted, adding Zn particles, preserving heat until the Bi particles are completely melted, adjusting the heating temperature to 400-420 ℃, and standing and preserving heat for 20-40 minutes.
8. The method of preparing a particle-reinforced high specific heat transfer alloy as claimed in claim 6, wherein the water-soluble auxiliary agent comprises: 1.5-2wt.% of succinic acid, 1.0-1.5wt.% of adipic acid, 0.5-1wt.% of salicylic acid, and the balance of ethanol.
9. The method of producing a particle reinforced high specific heat transfer alloy according to claim 6, wherein the mass fraction of the water soluble auxiliary agent is 18-20wt.% of the composite alloy powder.
10. The method for preparing a particle reinforced high specific heat transfer alloy according to claim 6, wherein the remelting is carried out in an inert atmosphere at 140 to 160 ℃ for 10 to 20 minutes for 2 to 3 times.
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| US20120153216A1 (en) * | 2010-12-21 | 2012-06-21 | Matthew Wrosch | High Transverse Thermal Conductivity Fiber Reinforced Polymeric Composites |
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| US20200001406A1 (en) * | 2017-11-22 | 2020-01-02 | Shenzhen Fitech Co., Ltd. | Micro/nano particle reinforced composite solder and preparation method therefor |
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| US20200335470A1 (en) * | 2019-04-22 | 2020-10-22 | Panasonic Corporation | Bonded structure and bonding material |
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| US20120153216A1 (en) * | 2010-12-21 | 2012-06-21 | Matthew Wrosch | High Transverse Thermal Conductivity Fiber Reinforced Polymeric Composites |
| CN106282734A (en) * | 2016-08-26 | 2017-01-04 | 杭州龙灿液态金属科技有限公司 | There is low melting point phase-change accumulation energy alloy, preparation technology and the application of high heat conductance |
| US20200001406A1 (en) * | 2017-11-22 | 2020-01-02 | Shenzhen Fitech Co., Ltd. | Micro/nano particle reinforced composite solder and preparation method therefor |
| US20200335470A1 (en) * | 2019-04-22 | 2020-10-22 | Panasonic Corporation | Bonded structure and bonding material |
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