CN113957285B - Preparation method of composite material - Google Patents
Preparation method of composite material Download PDFInfo
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- CN113957285B CN113957285B CN202111276796.XA CN202111276796A CN113957285B CN 113957285 B CN113957285 B CN 113957285B CN 202111276796 A CN202111276796 A CN 202111276796A CN 113957285 B CN113957285 B CN 113957285B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3732—Diamonds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3735—Laminates or multilayers, e.g. direct bond copper ceramic substrates
Abstract
The invention discloses a preparation method of a composite material, which comprises the following steps of orderly arranging diamond particles on the upper surface of a substrate layer to obtain a laminated material; stacking the stacked materials layer by layer to obtain a pre-pressing piece; pressurizing the pre-pressing piece by adopting a pressing die so as to press the diamond particles into the base material layer to obtain a semi-finished product I; filling gaps between pits and diamond particles generated when the diamond particles on the surface of the semi-finished product I are pressed into the substrate layer with the material of the substrate layer to obtain a semi-finished product II; and sintering the semi-finished product II, and then grinding to expose the diamond particles on the topmost layer, wherein the diamond particles on the topmost layer and the substrate layer are combined to form a flat surface so as to obtain a finished product. According to the invention, the diamond particles are orderly and uniformly distributed on the surface and in the composite material, the composite material with a large-size structure can be efficiently manufactured, the heat conduction uniformity is ensured, the processing is convenient, the efficiency is high, and the cost is low.
Description
Technical Field
The invention relates to the technical field of preparation of heat conduction materials, in particular to a preparation method of a composite material.
Background
Diamond is the substance with the highest thermal conductivity in nature, and the thermal conductivity at normal temperature is 2200 to 2600W/(m.K), and a coefficient of thermal expansion of about 0.86X 10 -6 And is an insulator at room temperature. Copper metal has high thermal conductivity, low cost, easy processing, and is the most commonly used packaging material, with a thermal conductivity of 400W/(m.K) and a thermal expansion coefficient of 17X 10 －6 And the material meets the use performance requirements of low thermal expansion coefficient and high thermal conductivity of the electronic packaging substrate material. Therefore, the diamond/copper composite material taking diamond as the reinforcing phase and copper as the matrix material has better heat conduction potential. The existing diamond/copper composite material has two modes of solid phase forming and liquid phase forming, and is prepared by controlling conditions such as temperature, time, pressure and the like, and common preparation methods comprise a high-temperature high-pressure method, a discharge plasma sintering method, a powder metallurgy method, a liquid phase infiltration method and the like, the process is complex, the implementation difficulty is high, the equipment is complex, the investment cost is high, and the distribution condition of diamond in the obtained diamond/copper composite material is random and uncontrollable, namely, the diamond serving as a reinforcing phase is unevenly distributed in a base material, the internal interfaces of the composite material are many and complex, the efficient transfer of heat is hindered, the local thermal conductivity of the composite material is poor, and the improvement of the thermal conductivity of the composite material is limited.
Disclosure of Invention
The invention aims to solve the technical problems and the technical task of improving the prior art, and provides a preparation method of a composite material, which solves the problems that in the prior art, the diamond of the composite material is unevenly distributed in a matrix material, so that the local heat conduction of the composite material is poor, and the overall heat conduction performance is influenced.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a method for preparing a composite material comprises the following steps:
sequentially arranging a layer of diamond particles on the upper surface of the base material layer to obtain a laminated material;
stacking the stacked materials layer by layer for a plurality of layers to obtain a pre-pressing piece;
pressurizing the prepressing piece by adopting a pressing die so as to press the diamond particles into the substrate layer to obtain a semi-finished product I;
filling gaps between pits and diamond particles generated when the diamond particles on the surface of the semi-finished product are pressed into the substrate layer by adopting the material of the substrate layer to obtain a semi-finished product II;
sintering the semi-finished product II to obtain a semi-finished product III;
and grinding the semi-finished product III to expose the diamond particles on the topmost layer and combine the diamond particles on the topmost layer with the substrate layer to form a flat surface, so as to obtain the finished composite material.
The composite material preparation method of the invention firstly arranges the diamond particles on the surface of the substrate layer in order, and then leads the diamond particles to be directly embedded and fixed on the substrate layer by pressure, thereby leading the diamond particles in the composite material to achieve the condition of ordered and uniform distribution, effectively improving the heat conduction uniformity of the composite material, avoiding uneven heat conduction caused by the diamond particles concentrated on the part of the substrate layer, conveniently and flexibly controlling the volume fraction of the diamond particles in the composite material, further flexibly adjusting the heat conductivity of the composite material according to the requirement, and laminating a plurality of layers after the diamond particles are arranged on the substrate layer in order, thereby obtaining the composite material with large size and thickness by only one-time pressing operation, improving the preparation efficiency, realizing the preparation of the composite material with large size and thickness, ensuring the good heat conduction uniformity while increasing the preparation size and specification of the composite material, effectively connecting the diamond particles and the substrate layer by a pressing mode, effectively improving the interface bonding state of the diamond particles and the substrate layer, ensuring the high heat conduction performance of the prefabricated plate, effectively ensuring the contact of the diamond particles and the smooth contact with the substrate layer by the existing composite material surface processing method, thereby ensuring the smooth contact of the heat conduction material and the smooth and the formation of the composite device with the heat conduction device, and the heat conduction device with the highest grinding cost of the heat conduction material, and the heat conduction device, and the invention can be formed by the invention, further effectively increasing the direct contact area of the diamond particles and the heating device, thereby further improving the heat-conducting property fundamentally.
Further, when the semi-finished product II is sintered, the semi-finished product II is placed in a sintering mold for limiting the shape and size of the semi-finished product II to be sintered, the phenomenon that the semi-finished product II obtained is seriously deformed due to softening and deformation of the base material layer in the sintering process is avoided, the shape and size of the base material layer in the sintering process are stable, and the structure and size of the finally obtained composite material meet requirements.
Further, the sintering mold comprises a pressing plate, and the pressing plate presses the second semi-finished product along the stacking direction of the stacking material. Because semi-manufactured goods two have the substrate layer of a plurality of layers, the substrate layer hugs closely together each other through the pressure effect of embossing mold utensil, but adjacent substrate layer still separates, the mode through the sintering makes adjacent substrate layer fuse as a whole, but simply through the heating sintering, adjacent substrate layer is difficult to the abundant contact and fuses, the clearance appears in inside easily, the situation of gas pocket, the pressure effect that utilizes the clamp plate makes adjacent substrate layer more closely laminate, the sintering makes the substrate layer reach the state of semi-liquid, simultaneously under the pressure effect, adjacent substrate layer can be better the combination be in the same place, improve the fine and close degree of the combined material's that finally obtains the base member, improve the final combined material heat conductivility who obtains.
Furthermore, sintering the semi-finished product II is sintering in a vacuum environment or sintering in a gas protection environment, so that the diamond particles and the substrate layer are prevented from being oxidized in the sintering process, the sintering quality is guaranteed, and the composite material has good heat-conducting property.
Further, after the layer of diamond particles are orderly arranged on the upper surface of the base material layer, a pressing die is adopted for pre-pressing so as to pre-embed the diamond particles on the surface of the base material layer, and then the laminated material is obtained. Diamond particles are embedded into the surface of the base material layer in advance, namely, the diamond particles and the base material layer are connected in advance, so that the state that the diamond particles are orderly arranged on the upper surface of the base material layer is maintained, the diamond particles are overlapped layer by layer, the position of the diamond particles can be prevented from shifting during stacking, the diamond particles which are evenly and orderly arranged in the whole three-dimensional space are ensured to be finally obtained, and the integral heat conduction uniformity of the composite material with large size specifications is improved.
Further, the diamond particles are orderly arranged on the surface of the base material layer through the distributing device, a plurality of cloth holes matched with the particle size of the diamond particles are formed in the distributing device, the cloth holes are orderly arranged along the surface of the base material layer, and each cloth hole only contains one diamond particle. The distribution situation of distributing hole is required diamond particle distribution situation on the substrate layer promptly on the distributing device, utilizes the distributing device can be reliable and accurate arrange the surface of substrate layer in order as required with diamond particle, distributing device simple structure, implementation cost are low, convenient to use, efficient.
Furthermore, the distributing hole is a slotted hole, an air hole communicated to the distributing hole is formed in the distributing device, and the caliber of the air hole is smaller than the grain diameter of the diamond particles and is used for being connected with a negative pressure device. Adsorb diamond particles in the cloth hole through the mode of negative pressure adsorption, the distributing device removes to the upper surface of substrate layer, then negative pressure device closes, and diamond particles can fall automatically and arrange in order on the surface of substrate layer as required, convenient to use, efficient, and the realization of being convenient for is automatic.
Further, arrange diamond particles on the sticky tape in order through the distributing device earlier, then with diamond particles face towards substrate layer surface's mode with the sticky tape attached to the substrate layer on, the embossing mold utensil carries out the pre-compaction in order to imbed diamond particles in advance on the surface of substrate layer, then removes the sticky tape in order to obtain the lamination. Utilize the viscidity of sticky tape to come the pre-fixing diamond granule to keep the state that diamond granule arranged in order, diamond granule through the pre-compaction and on the pre-embedding substrate layer, because the existence of sticky tape, can keep diamond granule position stable and the skew can not appear, and then make arranging the substrate layer as required that diamond granule can be accurate, improve diamond granule distribution accuracy nature.
Further, when the prepressing piece is pressurized by adopting a pressing die so as to press the diamond particles into the substrate layer, the pressing head of the pressing die is pressed down to the adjacent substrate layer to be attached together, and the pressing head is flush with the upper surface of the substrate layer at the topmost layer, so that the diamond particles can be fully embedded into the substrate layer, the diamond particles are fully combined with the substrate layer, the adjacent substrate layers can be fully fused into a whole when the follow-up sintering is ensured, the boundary between the adjacent substrate layers is eliminated, and the density of the finally obtained composite material is improved.
Furthermore, the mode of filling the gaps between the pits and the diamond particles generated when the diamond particles on the surface of the semi-finished product are pressed into the substrate layer by adopting the material of the substrate layer comprises one of a first method, a second method and a third method;
the method comprises the steps that a material of a base material layer is thermally sprayed to the surface of a semi-finished product I to obtain a semi-finished product II;
coating the material of the powdery base material layer on the surface of the semi-finished product I to obtain a semi-finished product II;
and the third method comprises the step of immersing the semi-finished product I into the liquid of the molten base material layer for a preset time and then extracting the semi-finished product I to obtain a semi-finished product II.
The density of the filler formed in the gap by the method I and the method II is low, the filler can be fully integrated with the substrate layer after the subsequent sintering step, the interface condition of the composite material is optimized, the composite material can form a continuous and flat surface conveniently, so that the contact area of the composite material and a heating device is increased, and the heat conduction effect is effectively improved.
A composite material is prepared by the preparation method of the composite material. The composite material is provided with the diamond particles which are orderly arranged on the surface, and the diamond particles which are orderly arranged are also arranged inside the composite material, so that the uneven heat conduction caused by the fact that the diamond particles are concentrated on the local part in the base material layer is avoided, the heat conduction uniformity of the composite material is effectively improved, the diamond particles are exposed on the surface of the composite material, the diamond particles can be effectively contacted with a heating device, the contact area between the diamond particles and the heating device is effectively increased, and the heat conduction performance is improved.
Compared with the prior art, the invention has the advantages that:
the preparation method of the composite material enables the diamond particles to be orderly and uniformly distributed on the surface and inside of the composite material, can efficiently prepare the composite material with a large-size structure, ensures the heat conduction uniformity of the composite material, enables the diamond particles to be exposed on the surface of the composite material, enables the diamond particles to be effectively contacted with a heating device, increases the contact area of the diamond particles and the heating device, improves the heat conduction performance, meets the requirements of various applications, enables the heat conduction rate of the composite material to reach 600-1000W/(m.K), is convenient to process, high in efficiency, low in cost, convenient to implement and free of complex equipment.
Drawings
FIG. 1 is a schematic structural view of a pressing die and a material distributor according to the present invention;
FIG. 2 is a schematic view of a pressing die and another material distributor according to the present invention;
FIG. 3 is a schematic view of a plurality of layers of a layered material stacked layer by layer to form a preform;
FIG. 4 is a schematic view of an induction heating coil arranged on a pressing mold for hot pressing;
FIG. 5 is a schematic view of the indenter pressing down to press the diamond particles into the substrate layer;
FIG. 6 is a schematic illustration of the topmost diamond particles pressed into the substrate layer to form pits;
FIG. 7 is a schematic view of filling the gap between the pits and the diamond particles with a material of the substrate layer;
FIG. 8 is a schematic diagram of the second semi-finished product placed in a sintering mold for sintering;
FIG. 9 is a schematic structural view of a composite material;
FIG. 10 is a schematic view of diamond particles being arranged on a tape using a distributor;
FIG. 11 is a schematic view of an adhesive tape attached to a substrate layer to pre-embed diamond particles into the substrate layer
FIG. 12 is a schematic structural view of a second semi-finished product pressed by a pressing plate arranged in a sintering mold.
In the figure:
the device comprises a base body 1, a base material layer 2, diamond particles 3, a laminated material 23, a distributor 4, a distribution hole 41, an air hole 42, a base 5, a pressure head 6, an induction heating coil 7, a sintering mold 8 and a pressing plate 81.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
According to the preparation method of the composite material disclosed by the embodiment of the invention, the diamonds are orderly and uniformly distributed on the base material, so that the heat conduction uniformity of the composite material is improved, the interface bonding state of the composite material is effectively improved, the interface thermal resistance is reduced, the overall heat conductivity of the composite material is effectively improved, the implementation is convenient, and the cost is low.
Example one
As shown in fig. 1 to 8, a method for preparing a composite material includes the steps of:
s1, orderly arranging a layer of diamond particles 3 on the upper surface of a base material layer 2 to obtain a laminated material 23;
specifically, the diamond particles 3 are orderly arranged on the upper surface of the substrate layer 2 through a distributor 4, the distributor 4 is provided with a plurality of distribution holes 41 matched with the particle sizes of the diamond particles 3, the distribution holes 41 are orderly arranged along the surface of the substrate layer 2, and each distribution hole 41 accommodates one diamond particle 3;
the distributing device 4 has two structures, as shown in fig. 2, one structure is that a distributing hole 41 is a through hole penetrating through the upper surface and the lower surface of the distributing device 4, the distributing device 4 is identical to a screen and the substrate layer 2 is flatly placed, then the distributing device 4 is placed on the upper surface of the substrate layer 2, then the diamond particles 3 are laid on the distributing device 4, the diamond particles 3 fall on the upper surface of the substrate layer 2 through the distributing hole, so that the diamond particles 3 are uniformly distributed on the upper surface of the substrate layer 2, and then the redundant diamond particles 3 on the distributing device 4 and the distributing device 4 are removed; as shown in fig. 1, in another structure, the material distribution hole 41 is a slotted hole, the material distributor 4 is provided with an air hole 42 communicated to the material distribution hole 41, the caliber of the air hole 42 is smaller than the particle diameter of the diamond particles 3, the air hole 42 is connected with a negative pressure device, the diamond particles 3 are adsorbed in the material distribution hole 41 through negative pressure, then the material distributor 4 is placed on the upper surface of the substrate layer 2, the negative pressure device stops, the diamond particles 3 automatically fall onto the upper surface of the substrate layer 2, the same diamond particles 3 are uniformly distributed on the upper surface of the substrate layer 2, the distribution efficiency and the precision of the diamond particles 3 by the material distributor 4 are high, the diamond particles 3 can be ensured to be orderly and uniformly distributed on the surface of the substrate layer 2 according to requirements, the finally obtained composite material is ensured to have the uniformly distributed diamond particles 3, and the heat conduction uniformity of the composite material is ensured;
the method for arranging the diamond particles 3 on the upper surface of the substrate layer 2 includes a specific method, as shown in fig. 10 and fig. 11, the diamond particles 3 are sequentially arranged on a tape 43 through a distributor 4, due to the viscosity of the tape 43, the diamond particles 3 can be adhered and fixed on the tape 43, and the distribution condition of the sequential arrangement is effectively maintained, then the tape 43 is attached to the surface of the substrate layer 2 in a manner that the diamond particles 3 face the surface of the substrate layer 2, due to the existence of the tape 43, the state of the sequential arrangement of the diamond particles 3 can be kept stable and unchanged, so that the diamond particles 3 can be pressed into the surface of the substrate layer 2 accurately in the follow-up process, it is ensured that the diamond particles 3 in the finally obtained composite material can be uniformly distributed in the sequential manner, after the tape 43 to which the diamond particles 3 are adhered is attached to the substrate layer 2, the subsequent step S2 can be directly performed, that the diamond particles 3 are pressed into the surface of the substrate layer 2 by using a pressing mold, but the pressure of the pressing process is very large, the tape 43 can be broken and remain on the diamond particles 3 and the substrate layer 2 and the organic matter can be removed by using a pre-pressing mold, and the pre-pressing method that the organic particles 3 are more preferably used for cleaning is a less, and the organic substrate layer 23, and the organic matter can be removed by using the pre-pressing method, and the pre-pressing method includes the pre-pressing method.
S2, superposing the laminated material obtained in the step S1 by a plurality of layers to obtain a pre-pressing piece;
the particle size of the diamond particles is usually very small, in this embodiment, a combination mode of directly pressing the diamond particles into the base material is mainly adopted, the diamond particles can only be pressed into the surface of the substrate layer 2, that is, the substrate layer 2 can only be distributed in the surface region of the substrate layer 2 and cannot directly go deep into the substrate layer 2, so the thickness of the single-layer substrate layer 2 cannot be too large, because the thickness of the substrate layer 2 is too large, the volume fraction of the diamond particles is very small, and further the overall thermal conductivity of the composite material is difficult to effectively improve, therefore, in order to improve the volume fraction of the diamond particles in the composite material, the composite material with a large-size structure is realized by adopting a laminated structure, the composite material with a large-size structure can be prepared, and meanwhile, the diamond particles can be uniformly distributed in the composite material, specifically, as shown in fig. 3, a first layer of substrate layer 2 is laid, then a first layer of diamond particles 3 is orderly arranged on the upper surface of the first layer of substrate layer 2, the first layer of substrate layer 2 and the first layer of diamond particles 3 are first layer laminated materials 23, then a second layer of substrate layer 2 is laid on the first layer of diamond particles 3, then a second layer of diamond particles 3 is orderly arranged on the upper surface of the second layer of substrate layer 2, and so on, a plurality of layers of laminated materials can be laminated, so that a pre-pressed piece with a certain height is finally obtained, and a finished composite material with a large-size structure obtained by performing subsequent treatment on the pre-pressed piece is obtained, wherein the thickness of the finished composite material is several times that of the single layer of substrate layer 2, and the finished composite material can be processed and cut to obtain various shapes and structures as required, so that the application range is wider;
moreover, the diamond particles 3 on the adjacent stacked materials are distributed in a staggered manner, that is, the connecting line of the diamond particles 3 on the adjacent stacked materials 23 is not perpendicular to the surface direction of the substrate layer 2, so that the diamond particles of the upper layer and the lower layer are prevented from colliding and contacting in the pressing process, the diamond particles are prevented from being broken due to compression, the integrity of the diamond particles is guaranteed, the thickness of the substrate layer is favorably reduced, the volume fraction of the diamond particles is effectively improved, and the thermal conductivity of the composite material is improved;
in this embodiment, the thickness of the substrate layer 2 is less than or equal to 10mm, the particle size of the diamond particles 3 is less than or equal to 5mm, preferably, the thickness of the substrate layer 2 is 0.1-1 mm, the particle size of the diamond particles 3 is 0.05-0.5 mm, substrate layers with different thicknesses and diamond particles with different particle sizes are flexibly selected, and the spacing between the diamond particles 3 distributed along the surface of the substrate layer 2 is controlled, so that the volume fraction of the diamond particles is flexibly controlled to adjust the overall thermal conductivity of the composite material, and various different requirements are met, the substrate layers 2 with the same thickness and the diamond particles 3 with the same particle size can be adopted as the stacked laminates 23, and the substrate layers 2 with different thicknesses or the diamond particles 3 with different particle sizes can also be adopted as the laminates, and specifically, the thickness of the substrate layer 2 on the topmost layer can be greater than that of the substrate layers 2 on the other layers, so that the diamond particles 3 in the finally obtained composite material are uniformly distributed in a three-dimensional space.
S3, pressurizing the pre-pressing piece by adopting a pressing die so as to press the diamond particles 3 into the substrate layer 2, thus obtaining a semi-finished product I;
the pressing die comprises a base 5 and a pressure head 6, the substrate layer 2 at the bottommost layer is flatly placed on the base 5, the pressure head 6 presses the base 5 downwards to press the diamond particles 3 into the substrate layer 2, the base material layer 2 is made of pure copper or copper-based composite material, the hardness of the base material layer is lower than that of the diamond particles 3, the pressure head 6 is made of material with hardness higher than that of the diamond particles 3, thereby ensuring the service life of the pressure head 6 and the pressing quality, the pressure head 6 of the pressing mould is provided with a plane parallel to the upper surface of the substrate layer 2, the pressure head of the pressing mould is pressed down to the adjacent substrate layers 2 and is jointed together, and the pressure head is flush with the upper surface of the topmost substrate layer 2, thereby completely pressing the diamond particles 3 into the surface of the substrate layer 2, and making the top of the diamond particles 3 at the topmost layer flush with the surface of the substrate layer 2, so that the diamond particles 3 and the substrate layer 2 can be fully combined, since the indenter 6 has a plane parallel to the upper surface of the base material layer 2 and the indenter 6 of the pressing mold is pressed down to be flush with the surface of the base material layer 2, so that all the diamond particles can be sufficiently embedded in the substrate layer 2 even if there is a deviation in the particle diameter of the diamond particles 3 arranged on the surface of the substrate layer 2, that is, the tops of all the topmost diamond particles are flush with the surface of the substrate layer 2, which is beneficial to ensuring the surface smoothness of the finally obtained composite material, ensuring the contact area between the composite material and a heating device when in use, improving the heat conduction effect, one plane of the surface of the diamond particle 3 at the topmost layer is flush with the surface of the base material layer 2, so that the exposed area of the diamond particle 3 is increased, the contact area of the diamond particle and a heating device is increased, and the heat conduction performance is improved;
in the pressing process, diamond particles between two adjacent substrate layers are embedded into the upper substrate layer and the lower substrate layer simultaneously, namely, the upper parts of the diamond particles are embedded into the lower surface of the upper substrate layer, the lower parts of the diamond particles are embedded into the upper surface of the lower substrate layer, so that a plurality of layers of laminated materials are connected into a whole after pressurization, when a pressure head of the pressing die presses down to the adjacent substrate layers 2 to be attached together, the diamond particles are fully wrapped by the upper substrate layer and the lower substrate layer, then the diamond particles and the substrate layers are more fully combined together through subsequent sintering, the adjacent substrate layers are also fused into a whole through sintering, the boundary is eliminated, the interface combination state of the composite material is optimized, the interface thermal resistance is reduced, and the overall thermal conductivity of the composite material is effectively improved.
The diamond particles 3 are single crystal particles, the shapes of the diamond particles include tetrahedrons, hexahedrons, octahedrons, dodecahedrons and the like, that is, the surfaces of the diamond particles 3 must have planes, as shown in fig. 6, when the topmost diamond particles 3 are embedded into the surface of the topmost substrate layer 2, one plane of the surface of the topmost diamond particles 3 is flush with the upper surface of the topmost substrate layer 2, that is, the exposed area of the topmost diamond particles 3 on the surface of the substrate layer 2 is increased to the maximum extent, so that the direct contact area of the diamond particles and a heating device is effectively increased, the heat conduction performance is effectively improved, the diamond particles 3 are hexahedrons, octahedrons and dodecahedrons, and the substrate layer 2 is a flat plate, when the diamond particles 3 are arranged on the surface of the substrate layer 2, the diamond particles 3 can be stably flatly placed on the surface of the substrate layer 2, that is, one plane of the diamond particles 3 is attached to the surface of the substrate layer 2 to achieve a stable flat state, at this time, the top surface of the diamond particles 3 is also a plane, the pressure head 6 is a plane parallel to the upper surface of the substrate layer 2, so that the pressure head 6 can ensure that the diamond particles 3 are pressed into the surface of the substrate layer 2 without rotating when pressed down, so that when the pressure head 6 is pressed down to be flush with the surface of the topmost substrate layer 2, the plane at the top of the diamond particles 3 is just flush with the lower surface of the pressure head 6, that is, the plane at the top of the diamond particles 3 is flush with the surface of the substrate layer 2, thereby facilitating the subsequent grinding treatment and polishing, ensuring that the top sides of all the diamond particles 3 are flat and the top sides of all the diamond particles 3 are just in the same plane when the diamond particles 3 are just exposed, the surface of the finally obtained composite material is smooth and flat, the exposure area of the diamond particles is effectively increased, the direct contact area of the diamond particles and a heating device is effectively increased, and the heat conducting performance is further effectively improved;
as shown in fig. 3 and 5, the pressing mold is used to directly press the diamond particles 3 into the surface of the substrate layer 2 in a cold pressing mode, that is, the pressing mold is used to press the diamond particles 3 into the surface of the substrate layer 2 by pressure, as shown in fig. 4, a hot pressing mode can also be used, that is, the substrate layer 2 is heated in the pressing process, the heating temperature is 400-1000 ℃, specifically, the base 5 can be provided with the induction heating coil 7 to heat the substrate layer 2, so that the material of the substrate layer 2 can be softened, the diamond particles 3 can be smoothly pressed into the surface of the substrate layer 2, and the diamond particles 3 can be better combined with the substrate layer 2, the interface combination state of the composite material is improved, and the heat conductivity is improved.
S4, filling gaps between pits and the diamond particles 3, which are generated when the diamond particles 3 on the surface of the semi-finished product one are pressed into the substrate layer 2, with the material of the substrate layer 2 to obtain a semi-finished product two;
when the diamond particles 3 at the topmost layer are pressed into the substrate layer 2, pits can be generated on the substrate layer, the diamond particles 3 are generally tetrahedral, hexahedral, octahedral, dodecahedral and the like, so that the caliber of the diamond particles 3 is large at the middle part and small at the two ends, the pits generated when the diamond particles 3 are pressed into the substrate layer 2 are matched with the middle part of the diamond particles 3, but are larger than the top part of the diamond particles 3, that is, after the diamond particles 3 are pressed into the surface of the substrate layer 2, gaps can be formed between the generated pits and the tops of the diamond particles 3, as shown in fig. 6, the gaps can seriously reduce the effective contact area of the composite material and a heating device, that is, the composite material is difficult to fully contact with the heating device, and the heat conduction effect is seriously affected, as a result, even if the volume fraction of the diamond particles in the composite material is increased, the actual heat conduction performance of the composite material is difficult to be improved, when the diamond particles 3 are pressed into the substrate layer 2, the pits can also extrude, so that the edges of the pits can be raised, the surface smoothness of the composite material can also be affected, and the effective contact area of the composite material with the heating device can be improved, and the effective contact area of the diamond particles 3 can be improved, and the effective contact condition of the composite material of the heat conduction interface of the composite material can be improved;
in the embodiment, the material of the substrate layer 2 is used for filling the gap between the pit and the diamond particle 3 generated when the diamond particle 3 on the upper surface of the semi-finished product is pressed into the substrate layer 2, so the material of the substrate layer 2 is used for filling, the material convenient for filling is sintered and then is integrated with the substrate layer 2, the interface complexity of the composite material is improved, and the heat conductivity is improved;
specifically, as shown in fig. 7, the manner of filling the gaps between the diamond particles 3 and pits generated when the diamond particles 3 on the surface of the semi-finished product are pressed into the substrate layer 2 with the material of the substrate layer 2 includes one of a first method, a second method, and a third method;
the first method comprises the steps of thermally spraying the material of the substrate layer 2 on the surface of the first semi-finished product to obtain a second semi-finished product;
the second method comprises the steps of coating the material of the powdery base material layer 2 on the surface of the first semi-finished product to obtain a second semi-finished product;
and the third method comprises the step of immersing the semi-finished product I into the liquid of the molten base material layer 2 for a preset time, and then extracting to obtain a semi-finished product II, wherein the liquid of the molten base material layer 2 can be rapidly immersed into and fill the gap between the pit on the semi-finished product I and the diamond particles, and the immersion time is 0.1-1 second.
S5, sintering the semi-finished product II to obtain a semi-finished product III;
sintering in a vacuum environment or in a gas-shielded environment, wherein the gas-shielded environment is an inert environment such as nitrogen or a reducing gas environment such as hydrogen or a mixed gas environment of nitrogen and hydrogen, the vacuum environment and the gas-shielded environment can effectively prevent the diamond particles and the substrate layer from being oxidized in the sintering process, adjacent substrate layers are fused together through sintering to eliminate the original boundary, and the filling material adopted in the method I and the method II in the S4 is fully combined with the substrate layer 2 into a whole, so that the interface combination state of the composite material is optimized, the heat transfer efficiency is improved, and the overall heat conduction performance of the composite material is improved, as shown in FIG. 8, the semi-finished product II is placed in a sintering mold 8 for sintering, and a plurality of sintering molds 8 can be accommodated in a sintering furnace simultaneously, each sintering mold 8 can be used for placing a single or a plurality of semi-finished products II, the sintering mold 8 is matched with the semi-finished products II in size, so that the size structure of the semi-finished products II is limited in the sintering process, the situation that the semi-finished products II are seriously deformed due to the softening and deformation of the base material layer 2 in the sintering process is avoided, the structure and the size of the finally obtained composite material meet requirements is ensured, the whole sintering mold 8 is a box body matched with the surface shape and the size of the base material layer 2, the edge of the semi-finished products II can be limited, the shape and the size of the obtained semi-finished products III meet the requirements, the middle part of the base material layer 2 can be arched and deformed in the sintering process, as shown in figure 12, a pressing plate 81 pressed on the surface of the base material layer 2 at the top layer is arranged in the sintering mold 8 to press the semi-finished products II, and particularly, the pressing plate presses the semi-finished products II along the laminating direction of the laminated materials, the pressure of clamp plate to semi-manufactured goods two is 10 ~ 50MPa, prevent that substrate layer 2 middle part from arching out of shape, further semi-manufactured goods two carries out the shape, spacing of size, improve the final composite's that obtains shape size precision, and, make the mutual inseparabler laminating of substrate layer in the semi-manufactured goods two through the pressure of clamp plate, promote the more effective integration together of substrate layer, eliminate the boundary between the substrate layer, avoid remaining the clearance in composite's inside, the gas pocket influences heat transfer efficiency, improve composite's heat conductivility, the temperature during sintering is 400 ~ 1300 ℃, ensure that the material of filling the clearance can effectively fuse with substrate layer 2 and become an organic whole, optimize the interface and combine the situation, the sintering time is 2 ~ 10min.
S6, grinding the semi-finished product III to expose the diamond particles 3 on the topmost layer and combine the diamond particles 3 on the topmost layer with the substrate layer 2 to form a flat surface, so as to obtain a finished composite material;
the surface of the semi-finished product III filled with the gaps is rough and uneven, and is difficult to fully and effectively contact with a heating device, so that the heat conduction performance is poor, and the diamond particles 3 are also covered by the filled material, so that the diamond particles 3 cannot directly contact with the heating device, and the heat conduction performance is influenced;
therefore, the semi-finished product II is ground and polished, the diamond particles 3 are fully exposed, the smoothness and the flatness of the surface of the composite material are improved, the composite material can be fully and well contacted with a heating device, the contact area is increased, the contact area of the diamond particles 3 and the heating device is large, the heat conducting performance is effectively improved, and the finished composite material is finally obtained.
The composite material prepared by the method is shown in fig. 9 and comprises a matrix 1 and diamond particles 3, wherein the matrix 1 is formed by sintering and fusing a plurality of layers of substrate layers 2, the matrix 1 is made of pure copper or copper-based composite material, the copper-based composite material is made of copper and doped with elements such as silver, aluminum, neodymium and the like, the diamond particles 3 which are orderly and uniformly distributed in a three-dimensional space are arranged in the matrix 1, the exposed diamond particles 3 are arranged on one surface of the matrix 1, the diamond particles 3 on the surface are orderly and uniformly distributed on the surface of the matrix 1, the diamond particles 3 on the surface and the surface of the matrix 1 are combined to form a smooth and flat surface, and further, one surface plane of the diamond particles 3 on the surface of the matrix 1 is flush with the surface of the matrix 1, so that the direct contact area of the diamond particles and a heating device is effectively increased, and the heat conduction performance is further effectively improved.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (10)
1. A method for preparing a composite material is characterized by comprising the following steps:
sequentially arranging a layer of diamond particles (3) on the upper surface of a base material layer (2) formed by a prefabricated plate to obtain a laminated material (23);
stacking the stacked material (23) layer by layer for a plurality of layers to obtain a pre-pressing piece;
pressurizing the pre-pressing piece by adopting a pressing die so as to press the diamond particles (3) into the substrate layer (2), wherein a pressing head 6 of the pressing die is a plane parallel to the upper surface of the substrate layer 2, the pressing head 6 is pressed down to be flush with the surface of the topmost substrate layer 2 so that the plane at the tops of the diamond particles 3 is flush with the surface of the substrate layer 2, the diamond particles (3) positioned between two adjacent substrate layers (2) are embedded into the upper substrate layer and the lower substrate layer (2) at the same time, and a first semi-finished product is obtained;
filling gaps between pits and the diamond particles (3) generated when the diamond particles (3) on the surface of the semi-finished product one are pressed into the substrate layer (2) by using the material of the substrate layer (2) to obtain a semi-finished product two;
sintering the semi-finished product II to obtain a semi-finished product III;
and grinding the semi-finished product III to expose the diamond particles (3) at the topmost layer and enable the top planes of the diamond particles (3) at the topmost layer to be flush with the surface of the base material layer (2) so as to form a flat surface in a combined mode, and thus the finished composite material is obtained.
2. The method for preparing the composite material according to claim 1, wherein when the second semi-finished product is sintered, the second semi-finished product is placed in a sintering mold for limiting the shape and the size of the second semi-finished product to be sintered.
3. The method for preparing a composite material according to claim 2, wherein the sintering mold comprises a pressing plate (81), and the pressing plate (81) presses the second semi-finished product along the stacking direction of the stacking material (23).
4. The method for preparing the composite material according to claim 1, wherein the sintering of the semi-finished product two is sintering in a vacuum environment or sintering in a gas protection environment.
5. The method for producing a composite material according to any one of claims 1 to 4, wherein after a layer of diamond particles (3) is arranged on the upper surface of the base material layer (2) in order, a pressing mold is used to perform pre-pressing to embed a part of the diamond particles (3) on the surface of the base material layer (2), and then the laminate (23) is obtained.
6. The preparation method of the composite material as claimed in any one of claims 1 to 4, wherein the diamond particles (3) are orderly arranged on the surface of the substrate layer (2) by a distributor (4), a plurality of distribution holes (41) matched with the particle size of the diamond particles (3) are formed in the distributor (4), the distribution holes (41) are orderly arranged along the surface of the substrate layer (2), and each distribution hole (41) only accommodates one diamond particle (3).
7. The preparation method of the composite material as claimed in claim 6, wherein the distribution holes (41) are slotted holes, the distributor (4) is provided with air holes (42) communicated with the distribution holes (41), and the caliber of the air holes (42) is smaller than the grain diameter of the diamond particles (3) and is used for connecting a negative pressure device.
8. The method for preparing a composite material according to claim 6, wherein the diamond particles (3) are sequentially arranged on the adhesive tape (43) through the distributor (4), then the adhesive tape (43) is attached to the substrate layer (2) in a manner that the diamond particles (3) face the surface of the substrate layer (2), the pressing mold is pre-pressed to pre-embed the diamond particles (3) on the surface of the substrate layer (2), and then the adhesive tape (43) is removed to obtain the laminate (23).
9. The method for preparing a composite material according to any one of claims 1 to 4, wherein the manner of filling the gaps between the diamond particles (3) and pits generated when the diamond particles (3) on one surface of the semi-finished product are pressed into the substrate layer (2) with the material of the substrate layer (2) comprises one of a first method, a second method and a third method;
the first method comprises the steps of thermally spraying the material of a substrate layer (2) on the surface of a first semi-finished product to obtain a second semi-finished product;
the second method comprises the steps of coating the material of the powdery base material layer (2) on the surface of the first semi-finished product to obtain a second semi-finished product;
and the third method comprises the step of immersing the semi-finished product I into the liquid of the melted material of the substrate layer (2) for a preset time, and then extracting the semi-finished product I to obtain a semi-finished product II, wherein the preset time is 0.1-1 second.
10. A composite material produced by the method for producing a composite material according to any one of claims 1 to 9.
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| CN102672188B (en) * | 2012-06-05 | 2015-01-21 | 安泰科技股份有限公司 | Method for positioning and distributing diamonds in tool bit and distributing device |
| CN105382263B (en) * | 2015-11-11 | 2017-05-24 | 东南大学 | Method for manufacturing ultrahigh-heat-conductive diamond-Al composite material with surface capable of being machined |
| CN111826542B (en) * | 2020-06-30 | 2022-01-04 | 长沙新材料产业研究院有限公司 | Copper-based diamond gradient heat dissipation material and preparation method thereof |
| CN112059192A (en) * | 2020-09-08 | 2020-12-11 | 泉州众志金刚石工具有限公司 | Production method for orderly arranging diamond sintered bodies |
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