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CN115637345B - Preparation method of composite material and composite material - Google Patents

Preparation method of composite material and composite material Download PDF

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Publication number
CN115637345B
CN115637345B CN202211082800.3A CN202211082800A CN115637345B CN 115637345 B CN115637345 B CN 115637345B CN 202211082800 A CN202211082800 A CN 202211082800A CN 115637345 B CN115637345 B CN 115637345B
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composite material
diamond
metal
microns
metal powder
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CN115637345A (en
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王郑
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Foshan Huazhi New Material Co ltd
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Foshan Huazhi New Material Co ltd
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Abstract

The application relates to a preparation method of a composite material and the composite material, and the method comprises the steps of filling diamond into filling holes of a metal framework to form a preform, wherein the pore diameter of the filling holes is larger than the particle diameter of the diamond. And hot-pressing the sintered preform to form the composite material. The diamond is filled into the filling holes of the metal framework, so that the strength of the composite material is enhanced by means of the metal framework, the thermal conductivity of the prepared composite material is improved by utilizing the characteristics of the diamond, and the thermal expansion coefficient of the composite material is reduced, so that the packaging requirement is met.

Description

Preparation method of composite material and composite material
Technical Field
The application relates to the technical field of semiconductor materials, in particular to a preparation method of a composite material and the composite material.
Background
With the development of semiconductor devices, the heat flux density of the semiconductor devices is continuously increased, and higher requirements are put on the heat dissipation performance of packaging materials. At present, some composite materials using diamond as a reinforcing body are difficult to meet the bonding strength requirement of the composite materials while guaranteeing the heat-radiating performance, and generally require a relatively complex preparation process.
Disclosure of Invention
Based on the above, the preparation method of the composite material and the composite material, which can simultaneously meet the heat dissipation requirement and the bonding strength requirement and have simple preparation process, are provided, so that the problems of lower bonding strength and complex preparation of the composite material are solved.
In one aspect of the present application, a method for preparing a composite material is provided, the method comprising:
filling diamond into the filling holes of the metal framework to form a preform; the pore diameter of the filling hole is larger than the particle diameter of the diamond;
and hot-pressing the sintered preform to form the composite material.
In one embodiment, the volume fraction of metal skeleton in the composite material is 10% -30%;
the volume fraction of diamond in the composite material is 30% -80%.
In one embodiment, the diamond has a particle size of 10 microns to 500 microns.
In one embodiment, the diamond includes a plurality of particle sizes.
In one embodiment, the hot press sintering of the preform to form the composite material further comprises:
filling metal powder into the filling holes of the metal framework; the particle size of the metal powder is smaller than the pore diameter of the filling pores.
In one embodiment, the volume fraction of metal powder in the composite is 10% -60%.
In one embodiment, the metal powder has a particle size of 5 microns to 200 microns; and/or
The metal powder includes a variety of particle sizes.
In one embodiment, the metal skeleton comprises a metal foam.
In one embodiment, the material of the metal skeleton comprises at least one of nickel, tungsten, molybdenum, cobalt, tantalum; and/or
The material of the metal powder comprises at least one of copper, silver, aluminum and nickel.
In another aspect of the application, a composite material is provided, and the composite material is prepared by the preparation method of the composite material.
According to the preparation method of the composite material and the composite material, the diamond is filled in the filling holes of the metal framework, so that the bonding strength of the composite material is enhanced by means of the metal framework, the thermal conductivity of the prepared composite material is improved by utilizing the characteristics of the diamond, and the thermal expansion coefficient of the composite material is reduced, so that the packaging requirement is met.
Drawings
FIG. 1 is a flow chart of a method of preparing a composite material according to an embodiment of the present application;
FIG. 2 is a flow chart of a method of preparing a composite material according to another embodiment of the present application.
Detailed Description
In order to make the above objects, features and advantages of the present application more comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application. This application is, however, susceptible of embodiment in many other forms than those described herein and similar modifications can be made by those skilled in the art without departing from the spirit of the application, and therefore the application is not to be limited to the specific embodiments disclosed below.
In the description of the present application, it should be understood that the terms "center," "longitudinal," "transverse," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," etc. indicate orientations or positional relationships based on the orientation or positional relationships shown in the drawings, are merely for convenience in describing the present application and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be configured and operated in a particular orientation, and therefore should not be construed as limiting the present application.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present application, the meaning of "plurality" is at least two, such as two, three, etc., unless explicitly defined otherwise.
In this application, unless specifically stated and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the terms in this application will be understood by those of ordinary skill in the art as the case may be.
In this application, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
It will be understood that when an element is referred to as being "fixed" or "disposed" on another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like are used herein for illustrative purposes only and are not meant to be the only embodiment.
Further, the drawings are not 1:1, and the relative dimensions of the various elements are drawn by way of example only in the drawings and are not necessarily drawn to true scale.
In order to facilitate understanding of the technical solutions of the present application, prior to the detailed description, a description will be first made of a composite material for packaging an existing semiconductor device.
As described in the background art, in recent years, the heat flux density of power devices such as silicon carbide and gallium nitride and high-power light emitting diodes has been increasing. The heat flux density is the heat transferred by the cross section of unit area in unit time, and is an important index for examining the heat dissipation performance of devices or equipment. The heat generated during operation of the device restricts further development of the device performance, so that the semiconductor device has higher requirements on the heat dissipation performance of the packaging material.
The inventor finds that the conventional metal packaging materials, such as copper, aluminum and other metal materials, have high thermal conductivity, but have high thermal expansion coefficient, and are difficult to match with chips and various packaging materials, so that the application of the conventional metal packaging materials is limited. In this regard, tungsten copper materials and kovar materials (iron-nickel-cobalt alloy materials) can form a better thermal expansion match with ceramic materials, semiconductor materials, metal materials and the like, but have lower thermal conductivity, and it has become increasingly difficult to meet the current high thermal conductivity requirements.
Diamond is a good heat dissipation packaging material due to the properties of high heat conductivity, low thermal expansion coefficient and low density, and has excellent application prospect in the field of semiconductors. However, since diamond has extremely high hardness, the surface is difficult to plate and process, and diamond with large size is difficult to prepare, complex in process, high in cost and difficult to process, diamond particles are usually compounded with metal materials such as aluminum, copper and silver, so that the packaging heat-dissipating material with high heat conductivity and low thermal expansion coefficient is obtained. The prepared packaging material has more competitive advantage in cost and can be better matched with the thermal expansion coefficients of the packaging materials such as kovar alloy, ceramic and the like.
In some related embodiments, diamond is typically used as a reinforcement, and a metallic or alloy material is combined with diamond particles to form a composite material. Wherein the reinforcement is the component of the composite material which bears the load. The inventor finds that, due to the large difference of thermal expansion coefficients between diamond and metal, the prepared composite material has lower bonding strength, and after high-low temperature circulation or long-term use, the bonding interface between diamond and metal has larger stress, and delamination or void generation is easy to occur, so that larger thermal resistance is generated, and further the heat dissipation performance of the composite material is degraded. In part of composite materials with metal materials as a matrix, high heat conductive materials, such as diamond-like layers, diamond layers, graphene and the like, are generally deposited on the surface of the composite materials, so that the cost is high and the yield is low. In addition, the metal substrate is used as an adhesion substrate of the high heat conduction material layer, and the deposition thickness of the high heat conduction layer is limited, so that the heat conduction effect is improved only to a limited extent.
Therefore, it is necessary to provide a preparation method of a composite material which can meet the heat dissipation requirement and the heat conduction requirement simultaneously and has a simple preparation process.
For convenience of description, the drawings show only structures related to the embodiments of the present application.
FIG. 1 shows a flow chart of a method of preparing a composite material in an embodiment of the present application.
In connection with some of the embodiments described below, it will be appreciated that the composite material is formed by machining a preform. The provided preform comprises a product form such as an intermediate state (i.e. a semi-finished product) or a final state (i.e. a finished product), the composite material comprises a product form such as an intermediate state (i.e. a semi-finished product) or a final state (i.e. a finished product), and the preform is an intermediate state of the composite material. That is, the composite material is derived from at least a portion of the preform. Since the embodiments of the present application claim emphasis on the methods involved in some embodiments described below, the specific structures and processes related to forming intermediate states or final states are not described here in detail.
Referring to fig. 1, a method for preparing a composite material according to an embodiment of the present application includes:
s110, filling diamond into the filling holes of the metal framework to form a preform; the pore diameter of the filling hole is larger than the particle diameter of the diamond;
s120, hot-pressing and sintering the preform to form the composite material.
In step S110, the "metal skeleton" refers to a solid skeleton made of metal, which is used as a reinforcement of the composite material to bear load, has a better supporting force, and ensures the strength of the composite material. "filling" means that diamond is allowed to enter the inside of the metal skeleton from the inside of the filling hole of the metal skeleton, so that the diamond and the metal skeleton can be reliably bonded together. Specifically, diamond refers to diamond particles, and the pore diameter of the filling hole is larger than the particle diameter of diamond, so that the diamond particles can easily enter the metal framework from the filling hole.
In step S120, "hot press sintering" refers to a sintering method in which the preform is heated while being pressurized, so that molding and sintering are simultaneously completed. In some embodiments, step S120 specifically includes placing the preform into a mold, and hot press sintering the preform and the mold to form the composite material. Illustratively, the material of the mold comprises graphite or ceramic.
According to the preparation method of the composite material, the filling holes of the metal framework are filled with the diamond, so that the strength of the composite material is enhanced by means of the metal framework, the thermal conductivity of the prepared composite material is improved by utilizing the characteristics of the diamond, and the thermal expansion coefficient of the composite material is reduced, so that the packaging requirement is met.
With continued reference to fig. 1, in some embodiments, step S110 may further include cleaning the metal skeleton and diamond. Thus, the surface dirt of the metal skeleton and the diamond can be removed by cleaning, and the bonding between the metal and the diamond is prevented from being hindered by the dirt. Specifically, the metal skeleton and the diamond are cleaned by an ultrasonic cleaning method. When ultrasonic waves with certain intensity are transmitted into the cleaning liquid medium, countless tiny bubbles are generated due to the alternate forward conduction of the ultrasonic waves, and the bubbles are formed and grown in a negative pressure area where the ultrasonic waves longitudinally propagate and are rapidly broken in a positive pressure area. This process of formation, growth, rapid collapse of microscopic bubbles is known as the "cavitation effect". In cavitation effect, the bubbles are broken to generate instantaneous high pressure exceeding 10000 atmospheres, and the cleaning liquid continuously bombards the surface of the object by means of the continuously generated instantaneous high pressure, so that dirt on the surface of the object is rapidly released, and a remarkable cleaning effect is achieved. Of course, in other embodiments, the cleaning may be performed by hand brushing, mechanical vibration, or the like, which is not limited thereto.
Alternatively, the cleaning solution may be deionized water or alcohol. Wherein deionized water refers to pure water from which impurities in the form of ions have been removed. Deionized water has a strong ion absorbing capacity and can pull ions from contaminants on the parts. It will be appreciated that deionized water is a very active cleaning agent in itself, and that deionized water provides better cleaning. In addition, metal ions affect the resistivity of the semiconductor, i.e., the yield of the semiconductor. Deionized water is selected to avoid the influence of ion impurities on semiconductors. The alcohol can reduce the loss of the crystal caused by dissolution, most of the inactive metals and alloys can not react with the alcohol, and after the soluble impurities and water on the surfaces of the metal framework and the diamond are removed, the metal framework and the diamond are easier to dry because the alcohol has the characteristic of easy volatilization. Of course, in other embodiments, the metal skeleton and the diamond surface may be cleaned with other solutions such as distilled water, which is not limited thereto.
The inventor researches that when the cleaning time is too short, the cleaning effect is poor, and dirt on the metal skeleton and the diamond surface is difficult to clean, and when the cleaning time is too long, the coating on the diamond surface can be fallen off under the action of ultrasonic waves, and the metal structure of the metal skeleton is also easy to damage. Based on this, in some embodiments, the cleaning time is 2 minutes to 10 minutes. It is understood that the cleaning time includes, but is not limited to, 2 minutes, 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, or 10 minutes.
Further, the method further comprises drying the metal framework and the diamond after cleaning the metal framework and the diamond. Therefore, the drying property of the metal framework and the diamond can be ensured, the bonding capability between the metal framework and the diamond is improved, the subsequent hot-pressing sintering efficiency is improved, and the preparation period is shortened. In some embodiments, after drying the metal skeleton and diamond, mixing the diamond and metal skeleton is also included. In this way, by mixing diamond with the metal skeleton, diamond can be filled into the metal skeleton. In particular to some embodiments, the diamond and metal skeleton are mixed by means of a ball mill. In this way, the ball mill can further ensure that the diamond fills more fully into the metal skeleton.
The inventor notes that in the process of preparing the composite material, the functions of each component are exerted to the greatest extent, and the influence on the performance of the composite material due to the excessive component of a certain component is avoided. When the content of diamond is too high, although the reduction of the thermal expansion coefficient and the improvement of the thermal conductivity are in favor of theory, the bonding strength of the composite material can be reduced due to the fact that the bonding force of the diamond and the metal framework is poor, cracks can be generated at the bonding interface, and the heat transfer and the thermal conductivity can be affected. When the content of the metal framework is too high, the bonding strength of the composite material is ensured, but the bonding strength is limited by the thermal conductivity of the metal framework, so that the thermal conductivity of the composite material is reduced. Based on this, in some embodiments, the volume fraction of metal skeleton in the composite is 10% -30%. The volume fraction of diamond in the composite material is 30% -80%. It is understood that the volume fraction of metal skeleton in the composite material includes, but is not limited to, 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, 26%, 28%, or 30%. The volume fraction of diamond in the composite material includes, but is not limited to, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, or 80%.
The inventors found in the research process that, although the larger particle diameter diamond has better heat conduction effect, the larger particle diameter diamond has higher preparation cost and material cost, and the bonding strength is difficult to meet the requirement. And diamond with too small particle size is difficult to effectively improve the thermal conductivity of the composite material. Based on this, in some embodiments, the diamond has a particle size of 10 microns to 500 microns. It is understood that the particle size of diamond includes, but is not limited to, 10 microns, 50 microns, 100 microns, 150 microns, 200 microns, 250 microns, 300 microns, 350 microns, 400 microns, 450 microns, or 500 microns.
Further, in order to obtain higher density, the performance of the composite material is improved, and the diamond comprises various particle sizes. It is understood that the various particle sizes refer to the different particle sizes of diamond. Illustratively, diamond having a particle size of 10 microns to 50 microns and 100 microns to 250 microns is selected. It is understood that the particle size of diamond includes, but is not limited to, 10 microns, 20 microns, 30 microns, 40 microns, 50 microns, 100 microns, 110 microns, 120 microns, 130 microns, 140 microns, 150 microns, 160 microns, 170 microns, 180 microns, 190 microns, 200 microns, 210 microns, 220 microns, 230 microns, 240 microns, or 250 microns. The diamond particle sizes herein are only illustrative of the use of diamond particles of different sizes, and diamond particles of different sizes may be selected as desired, and are not limited herein.
In some embodiments, the metal skeleton comprises a metal foam. The metal foam is a metal material composed of fine bubbles filled with air holes in a large volume proportion. These pores may be connected closed cells, known as metal foam. Or an unconnected network (open cells), known as a porous metal. The metal foam not only has higher thermal conductivity, but also has higher strength. In addition, in the process of preparing the metal foam, the size of the pore diameter and the occupancy of the pores of the metal foam can be controlled as required. In still other embodiments, the metal framework may also be a metal mesh, without limitation.
In some embodiments, the material of the metal skeleton comprises at least one of nickel, tungsten, molybdenum, cobalt, tantalum. On the one hand, the metal material belongs to refractory metals, and has a high melting point. On the other hand, the coefficient of thermal expansion of the metal is low, and the coefficient of thermal expansion of the composite material can be further reduced. In yet another aspect, the strength of the metal is relatively high, thereby enabling the strength of the composite material to be increased.
Fig. 2 shows a flow chart of a method of preparing a composite material according to another embodiment of the present application.
As shown in fig. 2, another embodiment of the present application provides a method for preparing a composite material, including:
s210, filling metal powder into the filling holes of the metal framework; the particle size of the metal powder is smaller than the pore diameter of the filling hole;
s220, filling diamond into the filling holes of the metal framework to form a preform; the pore diameter of the filling hole is larger than the particle diameter of the diamond;
s230, hot-pressing and sintering the preform to form the composite material.
In step S220 and step S230, the content in the foregoing embodiments may be specifically referred to, and will not be described herein. It should be noted that, in the embodiment of the present application, the filling holes of the metal skeleton are filled with the metal powder and the diamond at the same time to form the preform in the step S210 and the step S220 are not in a predetermined order. In other embodiments, the metal powder may be filled into the filling hole of the metal skeleton, and then diamond may be filled into the metal skeleton filled with the metal powder to form the preform, or the diamond may be filled into the filling hole of the metal skeleton, and then the metal powder may be filled into the metal skeleton filled with diamond to form the preform, which is not limited herein.
According to the preparation method of the composite material in the embodiment, the metal powder can be filled between gaps of the diamond and the metal framework, so that the bonding strength and the heat conductivity between the diamond and the metal framework are improved.
In some embodiments, step S210 is preceded by cleaning the metal skeleton, diamond, and metal powder. Thus, the surface dirt of the metal skeleton, diamond and metal powder can be removed by cleaning, and the bonding between the metal and the diamond is prevented from being hindered by the dirt. Specifically, the metal framework, the diamond and the metal powder are cleaned by an ultrasonic cleaning method. When ultrasonic waves with certain intensity are transmitted into the cleaning liquid medium, countless tiny bubbles are generated due to the alternate forward conduction of the ultrasonic waves, and the bubbles are formed and grown in a negative pressure area where the ultrasonic waves longitudinally propagate and are rapidly broken in a positive pressure area. This process of formation, growth, rapid collapse of microscopic bubbles is known as the "cavitation effect". In cavitation effect, the bubbles are broken to generate instantaneous high pressure exceeding 10000 atmospheres, and the cleaning liquid continuously bombards the surface of the object by means of the continuously generated instantaneous high pressure, so that dirt on the surface of the object is rapidly released, and a remarkable cleaning effect is achieved. Of course, in other embodiments, the cleaning may be performed by hand brushing, mechanical vibration, or the like, which is not limited thereto.
Alternatively, the cleaning solution may be deionized water or alcohol. Wherein deionized water refers to pure water from which impurities in the form of ions have been removed. Deionized water has a strong ion absorbing capacity and can pull ions from contaminants on the parts. It will be appreciated that deionized water is a very active cleaning agent in itself, and that deionized water provides better cleaning. In addition, metal ions affect the resistivity of the semiconductor, i.e., the yield of the semiconductor. Deionized water is selected to avoid the influence of ion impurities on semiconductors. The alcohol can reduce the loss of the crystal caused by dissolution, most of inactive metals and alloys can not react with the alcohol, and after the soluble impurities and water on the surfaces of the metal framework, the diamond and the metal powder are removed, the metal framework, the diamond and the metal powder are easier to dry because the alcohol has the characteristic of easy volatilization. Of course, in other embodiments, the metal skeleton, diamond and metal powder surface may be cleaned with other solutions such as distilled water, which is not limited herein.
The inventor researches that when the cleaning time is too short, the cleaning effect is poor, and dirt on the surfaces of the metal framework, the diamond and the metal powder is difficult to clean, and when the cleaning time is too long, the coating on the surface of the diamond can be fallen off under the action of ultrasonic waves, and the metal structures of the metal framework and the metal powder are also easy to damage. Based on this, in some embodiments, the cleaning time is 2 minutes to 10 minutes. It is understood that the cleaning time includes, but is not limited to, 2 minutes, 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, or 10 minutes.
Further, the method further comprises the step of drying the metal framework, the diamond and the metal powder after cleaning the metal framework, the diamond and the metal powder. Therefore, the drying property of the metal framework, the diamond and the metal powder can be ensured, the bonding capability among the metal framework, the diamond and the metal powder is improved, the subsequent hot-pressing sintering efficiency is improved, and the preparation period is shortened. In some embodiments, after drying the metal skeleton, diamond, and metal powder, mixing the diamond, metal skeleton, and metal powder is also included. In this way, by mixing the diamond, the metal skeleton and the metal powder, the diamond and the metal powder can be sufficiently and uniformly filled into the metal skeleton. In particular to some embodiments, diamond, metal skeleton and metal powder are mixed by means of a ball mill. Thus, the ball mill can further ensure that the diamond and the metal powder are more fully filled into the metal framework.
In some embodiments, step S230 specifically includes placing the preform into a mold, and hot press sintering the preform and the mold to form the composite material. Illustratively, the material of the mold comprises graphite or ceramic. In some embodiments, hot-pressing the preform and the mold to form the composite material specifically includes placing the mold with the preform in a heating furnace, introducing a gas while applying a predetermined pressure to the preform and heating to a predetermined temperature, and maintaining the temperature for a predetermined time to form the composite material. Further, the gas includes an inert gas and/or a reducing gas. Thus, whether the inert gas, the reducing gas or the mixed gas of the inert gas and the reducing gas, the oxidation reaction of the preform in the heating furnace can be prevented. Illustratively, the gas may be, but is not limited to, at least one of helium, neon, argon, krypton, xenon, nitrogen, hydrogen. Wherein, the heating furnace can be a sintering furnace.
The inventors have found that applying a large pressure to the preform can promote the interconnection between the components and reduce the voids, but that an excessive pressure can cause the structure of the components to be broken. Based on this, in some embodiments, the preset pressure is 20 megapascals to 300 megapascals. It is understood that the preset pressure includes, but is not limited to, 20 megapascals, 40 megapascals, 60 megapascals, 80 megapascals, 100 megapascals, 120 megapascals, 140 megapascals, 160 megapascals, 180 megapascals, 200 megapascals, 220 megapascals, 240 megapascals, 260 megapascals, 280 megapascals, or 300 megapascals.
The inventors have also found that, in combination with the particle size of the metal powder in some of the embodiments described below, the smaller the particle size of the metal powder, the more susceptible it is to atomic diffusion, the more susceptible it is to formation of a sintering neck, and thus the lower the sintering temperature is required. Moreover, if the sintering temperature is too high, not only is oxidation overburning easily generated, but also the too high temperature can accelerate the generation of some brittle phases of metal, so that the strength of the prepared composite material is reduced. Based on this, in some embodiments, the preset temperature is 0.6-0.9 times the melting point of the metal powder. It is understood that the preset temperature may be, but is not limited to, 0.6 times, 0.7 times, 0.8 times, or 0.9 times the melting point of the metal powder.
In some embodiments, hot press sintering the preform and the mold to form the composite material further includes maintaining the temperature for a predetermined time. In this way, the metal skeleton, diamond, and metal powder after mixing can be ensured to be sufficiently sintered and bonded. The inventor obtains that if the heat preservation time is too short, the metallurgical bonding among the metal framework, the diamond and the metal powder is insufficient, and the bonding strength requirement is difficult to reach through multiple experiments. The atomic diffusion and the formation of the sintering neck in metallurgical bonding are basically completed in a short time, and if the heat preservation time is too long, not only the obvious performance improvement can not be brought, but also the cost can be increased, and even the surface of the sintered composite material is further oxidized. Based on this, in some embodiments, the incubation time is 20 minutes to 120 minutes. It is understood that incubation times include, but are not limited to, 20 minutes, 30 minutes, 40 minutes, 50 minutes, 60 minutes, 70 minutes, 80 minutes, 90 minutes, 100 minutes, 110 minutes, or 120 minutes. Further, after the composite material is preserved for a preset time, the prepared composite material and the mold are cooled along with the furnace, and the cooled composite material can be taken out.
In connection with some of the foregoing embodiments, the inventors have noted that it is desirable to avoid excessive levels of certain components from affecting the performance of the composite while taking into account the full function of the components. While more metal powder may more fully fill the gaps between the diamond and the metal skeleton, thereby improving the bonding strength and thermal conductivity, too much metal powder may result in a too high coefficient of thermal expansion and a decrease in thermal conductivity. Based on this, in some embodiments, the volume fraction of metal powder in the composite is 10% -60%. It is understood that the volume fraction of metal powder in the composite material includes, but is not limited to, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, or 60%.
The inventor finds that the smaller the particle size of the metal powder is, the higher the surface free energy of the metal powder is, which is beneficial to promoting the atomic diffusion, so that the binding force, namely the binding strength of the composite material is improved. However, the metal powder having an excessively small particle diameter is liable to react with oxygen to form an oxide, and the oxide layer may hinder the diffusion of atoms, rather, the interlayer bonding force is lowered. Based on this, in some embodiments, the particle size of the metal powder is 5 microns to 200 microns. It is understood that the particle size of the metal powder includes, but is not limited to, 5 microns, 10 microns, 20 microns, 30 microns, 40 microns, 50 microns, 60 microns, 70 microns, 80 microns, 90 microns, 100 microns, 110 microns, 120 microns, 130 microns, 140 microns, 150 microns, 160 microns, 170 microns, 180 microns, 190 microns or 200 microns.
Further, in order to obtain higher density, the performance of the composite material is improved, and the metal powder comprises various particle sizes. It is understood that the plurality of particle sizes means that the particle sizes of the metal powders are different. Illustratively, metal powders having particle sizes of 5 microns to 30 microns and 80 microns to 150 microns are selected. It is understood that the particle size of the metal powder includes, but is not limited to, 5 microns, 10 microns, 15 microns, 20 microns, 25 microns, 30 microns, 80 microns, 85 microns, 90 microns, 95 microns, 100 microns, 105 microns, 110 microns, 115 microns, 120 microns, 125 microns, 130 microns, 135 microns, 140 microns, 145 microns, or 150 microns. The particle sizes of the metal powder are only illustrative, and the metal powder with different particle sizes can be selected according to the requirement, so that the method is not limited. In combination with the foregoing embodiments, diamond and metal powder with different particle sizes may be selected, diamond with different particle sizes may be selected, or metal powder with different particle sizes may be selected.
In some embodiments, the material of the metal powder includes at least one of copper, silver, aluminum, nickel. The metal material has good thermal conductivity, and the finally prepared composite material has higher thermal conductivity and can be more suitable for the field of semiconductor heat dissipation.
Based on the same inventive concept, on the other hand, the invention also provides a composite material, which is prepared by adopting the preparation method of the composite material. The composite material prepared by the preparation method has the advantages that the material inside the composite material is uniformly and isotropically distributed, the added metal framework effectively improves the strength of the material, and the inventor tests prove that the average tensile strength of the composite material is improved by 30-60 MPa compared with the average tensile strength of the composite material without the metal framework. In addition, the added metal framework can further reduce the thermal expansion coefficient of the composite material by selecting a metal material with a low thermal expansion coefficient, and the inventor tests that the thermal expansion coefficient is reduced by 0.2PPM/K-0.5PPM/K in the range of 25-200 ℃.
According to the preparation method of the composite material and the composite material, the diamond is filled into the filling holes of the metal framework, so that the strength of the composite material is enhanced by means of the metal framework, the thermal conductivity of the prepared composite material is improved by utilizing the characteristics of the diamond, the thermal expansion coefficient of the composite material is reduced, and the packaging requirement is met. In order to ensure that the components fully play roles and avoid the influence of the content of a certain component on the performance of the composite material, the volume fraction of a metal skeleton in the composite material is 10% -30%, the volume fraction of diamond is 30% -80% and the volume fraction of metal powder is 10% -60%. The diamond with the grain diameter of 10-500 microns and the metal powder with the grain diameter of 5-200 microns are selected, so that the heat conductivity of the composite material can be improved, and the bonding strength of the composite material can be ensured. And through diamond and metal powder with different particle diameters, higher density can be obtained, and the performance of the composite material is improved.
It should be noted that some of the technical solutions described above may be implemented as independent embodiments in the actual implementation process, or may be implemented as combined embodiments by combining them with each other. Some of the technical solutions described above are exemplary solutions, and specific how to implement the combination, and may be selected according to actual needs, and the embodiments of the present application are not limited specifically. In addition, in describing the foregoing embodiment of the present application, the different embodiments are described in a corresponding order based on the idea of convenience for description, for example, the order is preset according to the requirement in the actual implementation process, and the execution order of the different embodiments is not limited. Accordingly, in an actual implementation, if multiple embodiments provided in the embodiments of the present application need to be implemented, the execution order provided when the embodiments are set forth in the present invention is not necessarily required, but the execution order between different embodiments may be arranged according to the needs.
It should be understood that, although the steps in the flowcharts of fig. 1 and 2 are shown in order as indicated by the arrows, these steps are not necessarily performed in order as indicated by the arrows. The steps are not strictly limited to the order of execution unless explicitly recited herein, and the steps may be executed in other orders. Moreover, at least a portion of the steps in fig. 1 and 2 may include a plurality of steps or stages, which are not necessarily performed at the same time, but may be performed at different times, and the order of the execution of the steps or stages is not necessarily sequential, but may be performed in turn or alternately with at least a portion of the steps or stages in other steps or other steps.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples only represent a few embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the claims. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. Accordingly, the scope of protection of the present application is to be determined by the claims appended hereto.

Claims (10)

1. A method for preparing a composite material for use in the fabrication of a package structure for a semiconductor device, the method comprising:
filling metal powder into the filling holes of the metal framework; the particle size of the metal powder is smaller than the pore diameter of the filling hole;
filling diamond into the filling holes of the metal framework to form a preform; the pore diameter of the filling pores is larger than the particle diameter of the diamond;
and hot-pressing and sintering the preform to form the composite material.
2. The method of producing a composite material according to claim 1, wherein the volume fraction of the metal skeleton in the composite material is 10% to 30%;
the volume fraction of the diamond in the composite material is 30% -80%.
3. The method of preparing a composite material according to claim 1, wherein the diamond has a particle size of 10 to 500 microns.
4. The method of preparing a composite material according to claim 1, wherein the diamond comprises a plurality of particle sizes.
5. The method of producing a composite material according to any one of claims 1 to 4, wherein a preset pressure is applied to the preform during the hot press sintering, the preset pressure being 20 mpa to 300 mpa; and/or
And in the hot-pressing sintering process, heating the preform to a preset temperature which is 0.6-0.9 times of the melting point of the metal powder.
6. The method of producing a composite material according to any one of claims 1 to 4, wherein the volume fraction of the metal powder in the composite material is 10% to 60%.
7. The method of producing a composite material according to any one of claims 1 to 4, wherein the metal powder has a particle size of 5 to 200 μm; and/or
The metal powder includes a plurality of particle sizes.
8. The method of producing a composite material according to any one of claims 1 to 4, wherein the material of the metal skeleton includes at least one of nickel, tungsten, molybdenum, cobalt, tantalum; and/or
The material of the metal powder comprises at least one of copper, silver, aluminum and nickel.
9. The method of preparing a composite material according to any one of claims 1 to 4, wherein the metal skeleton comprises a metal foam.
10. A composite material prepared by the method of any one of claims 1-9.
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