CN108588456B - Cu-Sn intermetallic compound framework phase-change material and preparation method thereof - Google Patents
Cu-Sn intermetallic compound framework phase-change material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a Cu-Sn intermetallic compound skeleton reinforced phase change composite material and a preparation method thereof, wherein a continuous high-melting-point intermetallic compound skeleton structure and a low-melting-point alloy exist in the material, and the preparation method comprises the following steps: s1, preparing Cu-Sn-based alloy powder with a specific size; s2, carrying out surface treatment on the metal powder, and carrying out low-speed-high-speed secondary centrifugation; s3, mixing the two metal powders in proportion to obtain composite alloy powder; s4 is heated and compounded to obtain the Cu-Sn based phase change composite material with the intermetallic compound framework structure. The intermetallic compound skeleton in the composite material has high melting point (415-640 ℃), high mechanical strength (room temperature strength can reach 80MPa and high temperature strength at 250 ℃ can reach 40MPa) and good heat conduction and electric conductivity, and the composite material is low in cost, simple in preparation process and particularly suitable for being applied to the fields of heat-sensitive materials and electronic manufacturing as a thermal interface material or a packaging material.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a Cu-Sn intermetallic compound skeleton phase change material and a preparation method thereof.
Background
With the increasing demand of people for multi-functionalization and portability of electronic products, electronic information systems are continuously improved along the direction of miniaturization, high density and high performance, the integration level, the number of I/O pins and the power consumption of devices are continuously improved, and the thermal management problem of interconnection welding spots is increasingly prominent. When high-power equipment (such as a high-power LED, space electronics, automotive electronics and the like) works, the internal chip interconnection welding spot usually needs to bear the high temperature of more than 250-300 ℃, and for a new 3D high-density packaging technology, the greatly increased power density of a packaging system can also cause the further improvement of the working temperature in the system, so the heat resistance of the interconnection material becomes a key problem for determining the service performance and reliability of a high-power electronic device.
However, conventional lead-free solders such as Sn-Ag, Sn-Ag-Cu, Sn-Ag, etc. (melting point 150-; when the high-melting-point brazing filler metal is used, higher welding temperature is needed, and high-temperature damage to components is easily caused; the nano slurry is expensive and has too high cost, which can not meet the packaging requirements of high-power electronic devices.
For example, CN107096988A discloses a method for rapidly preparing an intermetallic compound Cu3Sn as an electronic packaging material: firstly, placing Sn foil and Cu foil into absolute ethyl alcohol for ultrasonic cleaning; secondly, coating flux paste on two surfaces of the cleaned Sn foil, and placing the Cu foil on the surface of the Sn foil to form a Cu/Sn/Cu sandwich structure foil; and thirdly, placing the Cu/Sn/Cu structural foil in the coil, pressing the surface of the foil by using a weight, controlling the heating temperature to be 240-530 ℃, controlling the brazing time to be 20-300 s, and continuously applying the pressure of 0.007-0.05 MPa for packaging. However, in order to obtain a uniform Cu3Sn intermetallic compound, the thickness of the Sn and Cu metal foils must be very thin, the preparation thereof is difficult and the process is very complicated; the solder paste in the foil type sandwich structure is not easy to volatilize, and large-area holes are easily formed in the obtained material, so that the preparation method provided by the invention cannot be widely applied to packaging and manufacturing of electronic products.
CN104625466A discloses a tin-based solder/copper particle composite solder capable of quickly forming high-temperature solder joints at low temperature, which is composed of tin-based solder powder, copper particle powder and flux paste. Wherein, the weight ratio of the tin-based solder powder to the copper particle powder is 5: 2 to 2: 3, the weight ratio of the residual soldering flux is 4-20%, the particle size of the tin-based solder powder is preferably 5-60 μm, and the particle size of the copper is preferably 0.1-10 μm. However, the volatilization and overflow of the flux under high temperature conditions easily cause a large number of holes to be formed inside the welding spot, and even if the welding spot is formed, the structural strength of the welding spot is often low due to loose material structure, and is generally only 30 MPa.
Therefore, the invention combines the advantages of high melting point characteristic of intermetallic compounds (IMC) and wide applicability of solder alloy to prepare the composite alloy, promotes the IMC framework with high strength and high melting point and the low melting point alloy to be formed inside the composite alloy, and improves the high-temperature structural stability and the high-temperature service performance of the material.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a Cu-Sn intermetallic compound framework phase-change material and a preparation method thereof, aims to obtain a lead-free composite material with excellent high-temperature structural stability and service performance, and solves the problems of poor high-temperature service performance, high cost and low reliability of the existing brazing filler metal and nano slurry.
The invention firstly provides a preparation method of a Cu-Sn based intermetallic compound skeleton reinforced phase change composite material, which comprises the following steps:
s1: respectively preparing Cu metal powder and Sn-based alloy powder with specific sizes;
s2: performing surface treatment on the two kinds of metal powder obtained in the step S1, and performing low-speed-high-speed secondary centrifugation;
s3: mixing the two metal powders obtained in the step S2 in proportion to obtain composite alloy powder;
s4: and (4) heating and compounding the composite alloy powder obtained in the step S3 to obtain the Cu-Sn based phase change composite material with the intermetallic compound framework structure.
The preparation steps and the processing method of the material are completely compatible with the preparation process of the existing electronic material, and can meet the industrial production requirement.
Particularly, compared with the commonly used gold-tin high-temperature solder, nano-silver paste and ultrasonic, electromagnetic induction and other full IMC welding spot preparation methods, the material provided by the invention has the advantages of simple preparation process, low material cost and process cost, strong process compatibility, more stable manufacturing yield and obvious application advantages.
In a further preferred embodiment, the Cu-Sn intermetallic compound skeleton-reinforced phase change composite material is one in which the high melting point intermetallic compound is Cu6Sn5、Cu3Sn or a mixture of the two, and the melting point range is 415-640 ℃.
In a further preferred embodiment, the Cu — Sn intermetallic compound skeleton-reinforced phase change composite material is a Sn-based alloy such as pure Sn, SAC alloy, and Sn — Cu alloy, and has a melting point range of 218-.
The above materials or structures have excellent material and process compatibility in the field of electronic manufacturing, the melting and electrothermal characteristics thereof are particularly suitable for the existing electronic products and devices, and the manufacturing and application costs thereof are lower compared with other common electronic materials such as Ni, Au, Ag, Ti, Cr, and the like.
Further preferably, in the preparation method of the Cu-Sn intermetallic compound skeleton-reinforced phase change composite material, in the step S1, the metal powder is prepared by a ball milling method, a laser method or a spray drying method, the average size of the Cu metal powder is 0.2 to 5 μm, the Sn-based alloy powder is an alloy such as pure Sn, Sn-Ag-Cu, Sn-Ag, and the like, the average size is 10 to 40 μm, and the particle diameter ratio of the two is 1: 5 to 20. The metal powder with the size characteristics is used for preparing the phase-change composite material, so that the contact and reaction area among materials can be increased to the maximum extent, the formation of an IMC framework structure along the surface of the Sn-based alloy powder is promoted, the problems of agglomeration, incapability of filling particle pores and the like are avoided, the Sn-based low-temperature phase still exists in the material, and the phase change at high temperature is realized.
In a further preferred embodiment, in the preparation method of the Cu-Sn intermetallic compound skeleton-reinforced phase change composite material, the surface treatment method of the powder in the step S2 is to perform acid washing by using one or a mixture of several of formic acid, acetic acid, hydrochloric acid, ethanol, acetone and the like, and then perform ultrasonic cleaning for many times by using deionized water or organic solvents such as ethanol, ethylene glycol, acetone and the like; or surface activation is carried out by using surfactants such as succinic acid, glutaric acid, abietic acid, dimethylamine hydrochloride and the like, wherein the molar ratio of acid to metal powder is 0.6-1.5: 1, and the mass ratio of the surfactant to the metal powder is 1-5: 100.
the treatment method can remove oxides on the surface of the metal powder, improve the activity of the metal powder, improve the reaction boundary condition and remove impurities, and promote the metal powder to form a complete IMC framework structure in a short time, thereby ensuring the high-temperature performance of the material; the above treatment method is effective and necessary because the problem of oxidation of the untreated metal powder is very serious and it is difficult to form effective bonding even under high temperature and high pressure conditions.
In a further preferable embodiment, in the step S2, the low-speed centrifugation rotation speed is not more than 1500rpm, the high-speed centrifugation is not more than 3000rpm, the upper suspension is retained after the low-speed centrifugation, and the precipitate is retained after the high-speed centrifugation. The method can further screen the metal powder and ensure the uniform particle size, thereby avoiding the problems of segregation, agglomeration, stress concentration and the like in the subsequent compounding process and ensuring the uniformity and reliability of the obtained composite material.
Further preferably, in the preparation method of the Cu-Sn intermetallic compound skeleton-reinforced phase change composite material, the mass ratio of the Cu metal powder in the step S3 is 20-55%. The mass ratio is the minimum content required for forming a continuous IMC structure confirmed by tests, and if the mass ratio is lower than 20%, the IMC phase quantity in the obtained composite material is insufficient and discontinuous, and the structural strength cannot be provided under the high-temperature condition; if it exceeds 55%, the sintering temperature of the Cu powder itself is extremely high, and the composite material is difficult to mold.
Further preferably, in the preparation method of the Cu-Sn intermetallic compound skeleton-reinforced phase change composite material, the composite mode of the composite alloy powder in the step S4 is reflux or hot pressing, the heating peak temperature is 200-. The above technological parameters can be completely compatible with the existing electronic manufacturing process, 200 ℃ is the lowest critical temperature for forming the composite material of the invention, and 60s is the necessary time for ensuring the full reaction of the metal powder; if the heating temperature, the heating time and the hot-pressing pressure are further increased, other parts or materials in the electronic product are easily damaged, or excessive reaction is caused, and a full IMC structure with high brittleness and poor heat conduction/electric energy is formed.
In addition, the invention provides a Cu-Sn intermetallic compound skeleton-reinforced phase-change composite material, which is prepared by the preparation method, wherein a continuous high-melting-point intermetallic compound skeleton structure and a low-melting-point alloy exist in the material, the whole structure can be kept stable under a high-temperature condition (250-600 ℃), and the low-melting-point alloy can be converted into a high-activity liquid structure.
The beneficial effects of the invention compared with the prior art comprise:
(1) the invention selects micron Cu and Sn base powder with specific size and proportion to prepare the Cu-Sn composite alloy with high temperature service performance based on the principle of minimum surface energy and the principle of surface adsorption. By removing the surface oxide of the metal powder, activating the surface, stirring and heating under the condition of being higher than the melting point of the Sn-based powder, the Cu powder with small grain diameter is promoted to be uniformly distributed at the interface between the large-size Sn-based powder to generate semi-solid metallurgical reaction, and a Cu-Sn intermetallic compound framework structure is formed.
(2) The intermetallic compound skeleton has high melting point (>410 ℃), high mechanical strength and good heat conduction and electric conductivity, and can maintain the integral stability of the material structure under the high-temperature condition. Meanwhile, through the size and proportion design, the large-size Sn-based powder cannot completely participate in metallurgical reaction, the residual unreacted part is used as a low-temperature phase change material to be present in the gap of an intermetallic compound framework, and the phase change materials are converted into liquid metal structures during high-temperature service (230 ℃), so that the deformability, the heat conduction and the electric conduction capability of the whole structure of the material are effectively improved.
(3) The material can be molded at a lower temperature, has good strength, electric conductivity, thermal conductivity and reliability at a high temperature, has a room-temperature shear strength of 60-80MPa, can maintain a shear strength of 20-40MPa at a high temperature of 250 ℃, has a lower cost, is completely compatible with the existing material preparation and processing processes, and is particularly suitable for being applied to the fields of heat-sensitive materials and electronic manufacturing as a thermal interface material or a packaging material.
Drawings
FIG. 1 shows Cu obtained in example 23Sn and Cu6Sn5Microstructure morphology of skeleton reinforced phase change composite material
FIG. 2 shows Cu obtained in example 36Sn5Microstructure morphology of skeleton reinforced phase change composite material
Detailed Description
The invention is explained below with reference to specific embodiments and the drawing, without being restricted thereto.
Example 1A Cu-Sn intermetallic compound skeleton phase change material having continuous Cu therein3The Sn skeleton structure and the low-melting-point pure Sn phase are prepared by the following steps:
(1) preparing Cu powder and Sn powder with average grain diameter of 2 microns and 40 microns respectively by a ball milling method;
(2) and carrying out deoxidation treatment on the two obtained metal powders by using a hydrochloric acid alcohol solution with the volume fraction of 3%, controlling the molar ratio of formic acid to the metal powders to be 1.2:1, carrying out ultrasonic cleaning for 3-4 times by using absolute ethyl alcohol, and then carrying out low-speed-high-speed secondary centrifugation at the rotating speeds of 500rpm and 1500rpm respectively for 3 minutes to obtain pure metal powder.
(3) Drying the two powders at 65 ℃ for 20 minutes under vacuum, adding glutaric acid and dimethylamine hydrochloride, and mixing by using a planetary stirrer to obtain uniform composite alloy powder, wherein the mass ratio of Cu to Sn is 55: 45, the total content of the surfactant is 3.5 percent, and the mass ratio of glutaric acid to dimethylamine hydrochloride is 3: 1.
(4) Heating the uniformly mixed composite alloy powder for 540s at 300 ℃ by using an infrared heating furnace, and carrying out forced convection cooling by using external air to obtain the alloy powder with Cu3The Cu-Sn based phase change composite material with the Sn intermetallic compound skeleton structure can keep stable structure at the temperature of below 600 ℃, has extremely low cost and has good strength, electric conduction and heat conduction capability.
Example 2A Cu-Sn intermetallic compound skeleton phase change material having continuous Cu therein3Sn and Cu6Sn5The preparation method of the mixed framework structure and the low-melting-point Sn-Ag phase comprises the following steps:
(1) preparing Cu powder and Sn-Ag powder with average grain diameters of 1.5 microns and 20 microns respectively by a ball milling method;
(2) and carrying out deoxidation treatment on the obtained metal powder by using a hydrochloric acid alcohol solution with the volume fraction of 3%, controlling the molar ratio of hydrochloric acid to the metal powder to be 0.9:1, carrying out ultrasonic cleaning for 3-4 times by using deionized water, and then carrying out low-speed-high-speed secondary centrifugation at the rotating speeds of 1000rpm and 2000rpm respectively for 3 minutes to obtain pure metal powder.
(3) Drying the two kinds of powder for 30 minutes at 50 ℃ under a vacuum condition, adding 2% abietic acid by mass, and performing ball milling again to obtain uniform composite alloy powder, wherein the mass ratio of Cu to Sn is 4: 6.
(4) heating the mixed composite alloy powder at 275 deg.C and 0.5MPa for 180s with infrared heating furnace, and air cooling in atmospheric environment to obtain the final product with Cu3Sn and Cu6Sn5A phase-change composite material with an intermetallic compound skeleton structure.
Wherein, Cu3Sn and Cu6Sn5The microstructure morphology of the skeleton-reinforced phase-change composite material is shown in FIG. 1.
The composite material can keep stable structure at 550 ℃, has excellent strength, electric conduction and heat conduction capability under the high-temperature condition, has room-temperature shear strength of 60MPa and high-temperature shear strength of 15-35MPa, and has the advantages of widest applicability and highest cost performance.
Example 3A Cu-Sn intermetallic compound skeleton phase change material having continuous Cu therein6Sn5A skeleton structure and low melting point SAC305 phase, which is prepared by a method comprising:
(1) preparing Cu powder and SAC305 powder having average particle diameters of 1 micron and 15 microns, respectively, by a spray drying method;
(2) washing the obtained metal powder by using a formic acid alcohol solution with the volume fraction of 4%, removing oxides, controlling the molar ratio of formic acid to the metal powder to be 0.8:1, then ultrasonically washing the metal powder by using absolute ethyl alcohol for 3 to 4 times, and performing low-speed-high-speed secondary centrifugation at the rotating speeds of 1000rpm and 2500rpm respectively for 4 minutes to obtain pure metal powder.
(3) The obtained Cu and Sn powders were dried under vacuum at 50 ℃ for 30 minutes, and then mixed at a mass ratio of 35:65, and stirred using a planetary stirrer to obtain a uniform composite alloy powder.
(4) Using a hot press at 260 ℃ and 1MPaHeating the uniformly mixed composite alloy powder for 60s, and cooling along with the furnace to obtain the alloy powder with continuous Cu6Sn5A phase-change composite material with an intermetallic compound skeleton structure.
Wherein, Cu6Sn5The microstructure morphology of the skeleton-reinforced phase-change composite material is shown in FIG. 2.
The composite material has the advantages of simple preparation process, quickest molding, compact material structure, capability of keeping stable structure at the temperature of below 420 ℃, room-temperature shear strength of 80MPa, 250- ℃ shear strength of 40MPa, and relatively high cost.
Comparative example 1
A Cu-Sn composite alloy material is prepared by the following steps:
(1) preparing Cu powder and Sn powder with the particle size of 10-20 microns by a spray drying method;
(2) mixing the two powders according to the mass ratio of 4:6, adding 9-13 mass percent of soldering flux, and uniformly stirring.
(3) And heating the uniformly mixed composite alloy powder for 60s at 280 ℃ and 0.5MPa by a reflux process, and cooling along with the furnace.
Under the process conditions of the embodiment, because the metal powder has larger space and is easy to oxidize, a compact composite alloy is difficult to obtain even though the soldering flux is used, only gray black and dispersed alloy powder is often formed, the strength is low and is only 20-30MPa, the heat conduction/electric conduction capability is insufficient and is easy to break under the high-temperature condition, and the performance of the composite material is far lower than that of the composite material disclosed by the invention.
Comparative example 2
A Cu-Sn composite material is prepared by the following steps:
(1) preparing Cu powder and SAC305 powder with average particle size of 100 nm and 5 μm by laser method;
(2) the obtained metal powder was cleaned with a formic acid alcohol solution with a volume fraction of 4%, and ultrasonically cleaned with anhydrous ethanol 3 to 4 times to obtain pure metal powder.
(3) The obtained Cu and Sn powders are dried for 30 minutes under the vacuum condition of 60 ℃, and then the two powders are mixed according to the mass ratio of 3:7 and are stirred uniformly.
(4) And heating the uniformly mixed composite alloy powder for 60s under the conditions of 30MPa and 280 ℃, and cooling along with the furnace to obtain the phase-change composite material.
Compared with other examples, the embodiment uses the nano material with higher activity, but the nano Cu powder is easy to agglomerate or segregate in the stirring and heating processes and cannot be uniformly dispersed in the composite material, large-size IMC particles are easy to form in the composite material after the preparation process is finished, and a continuous IMC framework structure is difficult to obtain, so that the shear strength of the composite material at the high temperature of 250 ℃ is reduced to only 1-5 MPa.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. The preparation method of the Cu-Sn-based intermetallic compound skeleton-reinforced phase-change composite material is characterized by comprising the following steps of:
s1: respectively preparing Cu metal powder with a specific size and low-melting-point Sn-based alloy powder with a melting point range of 218-240 ℃, wherein the metal powder is prepared by a ball milling method, a laser method or a spray drying method, the average size of the Cu metal powder is 0.2-5 mu m, the average size of the Sn-based alloy powder is 10-40 mu m, and the particle diameter ratio of the Cu metal powder to the Sn-based alloy powder is 1: 5-20;
s2: performing surface treatment on the two metal powders obtained in the step S1, performing low-speed-high-speed secondary centrifugation, performing acid washing through one or a mixture of more of formic acid, acetic acid and hydrochloric acid, wherein the molar ratio of acid to metal powder is 0.6-1.5: 1, and performing multiple ultrasonic cleaning through deionized water, ethanol, ethylene glycol or acetone; or surface activation is carried out by using surfactants of succinic acid, glutaric acid, abietic acid and dimethylamine hydrochloride, wherein the mass ratio of the surfactant to the metal powder is (1-5): 100, the low-speed centrifugation rotating speed is not more than 1500rpm, the high-speed centrifugation is not more than 3000rpm, the upper suspension is reserved after the low-speed centrifugation, and the precipitate is reserved after the high-speed centrifugation;
s3: mixing the metal powder obtained in the step S2 in proportion, wherein the mass ratio of the Cu metal powder is 20-55%, and obtaining composite alloy powder;
s4: and (4) heating and compounding the composite alloy powder obtained in the step S3, wherein the compounding mode is reflux or hot pressing, the heating peak temperature is 200-300 ℃, the heating time is 60-600S, the hot pressing pressure is 0-40MPa, and the cooling mode is air cooling, furnace cooling and air cooling, so that the Cu-Sn-based phase change composite material with the intermetallic compound framework structure is obtained.
2. The method of claim 1, wherein: the intermetallic compound is Cu6Sn5、Cu3Sn or a mixture of the two.
3. The method of claim 1, wherein: the low melting point Sn-based alloy powder is pure Sn, SAC alloy, Sn-Cu alloy or Sn-Ag alloy.
4. A Cu-Sn intermetallic skeleton-reinforced phase change composite material, characterized by being produced by the production method according to any one of the preceding claims 1 to 3.
5. The composite material as claimed in claim 4, wherein a continuous high melting point intermetallic compound skeleton structure and a low melting point alloy exist in the material, the whole structure can be kept stable under the high temperature condition of 250-600 ℃, and the low melting point alloy can be transformed into a high-activity liquid structure.
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| CN113025284B (en) * | 2021-03-12 | 2021-08-20 | 中国矿业大学 | Medium-high temperature nano composite metal phase change heat storage material and preparation method thereof |
| CN114700653A (en) * | 2022-04-13 | 2022-07-05 | 北京理工大学 | High-hardness all-intermetallic compound welding spot and preparation method thereof |
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| CN101519737A (en) * | 2008-02-28 | 2009-09-02 | 王广武 | Mixed powder alloy with high melting point particles or fibers and low melting point particles as well as method for preparing same |
| CN106077654A (en) * | 2016-07-29 | 2016-11-09 | 柳州豪祥特科技有限公司 | A kind of method preparing powdered metallurgical material |
| CN107096988A (en) * | 2017-05-11 | 2017-08-29 | 哈尔滨理工大学 | One kind quickly prepares electronic package material Cu3The method of Sn intermetallic compounds |
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| CN101519737A (en) * | 2008-02-28 | 2009-09-02 | 王广武 | Mixed powder alloy with high melting point particles or fibers and low melting point particles as well as method for preparing same |
| CN106077654A (en) * | 2016-07-29 | 2016-11-09 | 柳州豪祥特科技有限公司 | A kind of method preparing powdered metallurgical material |
| CN107096988A (en) * | 2017-05-11 | 2017-08-29 | 哈尔滨理工大学 | One kind quickly prepares electronic package material Cu3The method of Sn intermetallic compounds |
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