CN112968005B - Diamond compact with interconnected pores and method for manufacturing same - Google Patents

Diamond compact with interconnected pores and method for manufacturing same Download PDF

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Publication number
CN112968005B
CN112968005B CN202110142309.4A CN202110142309A CN112968005B CN 112968005 B CN112968005 B CN 112968005B CN 202110142309 A CN202110142309 A CN 202110142309A CN 112968005 B CN112968005 B CN 112968005B
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diamond
substrate
holes
hole
diamond film
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CN112968005A (en
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王�琦
王忠强
郑小平
梁智文
刘南柳
陶仁春
张国义
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Dongguan Institute of Opto Electronics Peking University
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    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26Deposition of carbon only
    • C23C16/27Diamond only
    • C23C16/274Diamond only using microwave discharges
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • C23C16/511Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using microwave discharges
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    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/48Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
    • H01L21/4803Insulating or insulated parts, e.g. mountings, containers, diamond heatsinks
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    • H01L21/48Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
    • H01L21/4803Insulating or insulated parts, e.g. mountings, containers, diamond heatsinks
    • H01L21/481Insulating layers on insulating parts, with or without metallisation
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    • H01L23/373Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
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    • H01L23/3733Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon having a heterogeneous or anisotropic structure, e.g. powder or fibres in a matrix, wire mesh, porous structures
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    • H01L23/373Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H01L23/3735Laminates or multilayers, e.g. direct bond copper ceramic substrates

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Abstract

The invention relates to the technical field of composite materials, in particular to a diamond compact with communicating holes and a manufacturing method thereof, which comprises the steps of firstly, manufacturing through holes penetrating through the upper surface and the lower surface of a substrate to form a substrate with holes; and respectively depositing and growing diamond films on the upper surface and the lower surface of the substrate with the holes and in the through holes of the substrate with the holes, and finally obtaining the diamond composite sheet. The invention provides a composite sheet with high hardness, high thermal conductivity, high insulation resistance, low dielectric constant and high chemical stability, which can be used as a substitute material of a polycrystalline diamond self-supporting sheet in many occasions.

Description

Diamond compact with interconnected pores and method for manufacturing same
Technical Field
The invention relates to the technical field of composite materials, in particular to a diamond compact with communicating holes and a manufacturing method thereof.
Background
Modern technology is rapidly developed, the power and integration degree of electronic devices are higher and higher, so that the heat production concentration is higher and higher, and the stability of the heat production of the devices on the work cannot be ignored. Therefore, how to efficiently and rapidly extract heat has become a focus of research in the industry. The preparation of high thermal conductivity materials is an essential part of the forward path of electronic devices.
In addition, the high frequency high power integrated circuit substrate needs high thermal conductivity, high electrical insulation property, low dielectric constant and high chemical stability to reduce the performance impact on the integrated circuit and prolong the service life of the product.
Disclosure of Invention
In order to solve the above problems, the present invention provides a diamond compact with interconnected pores, which can be used as a substitute material for a polycrystalline diamond self-supporting sheet in many cases due to its properties such as high hardness, high thermal conductivity, high insulation resistance, low dielectric constant, and high chemical stability, and a method for manufacturing the same.
In order to achieve the purpose, the invention adopts the technical scheme that: a diamond compact with interconnected pores and a manufacturing method thereof;
the diamond compact with the communicating hole comprises a substrate, wherein the substrate is provided with at least one through hole penetrating through the upper surface and the lower surface of the substrate; the diamond composite sheet with the communicating hole also comprises a diamond film which is deposited and grown on the upper surface and the lower surface of the substrate and the inner wall of the through hole.
Preferably, the diameter of the through hole is less than 0.4 mm; the diamond film completely fills the through hole to form a diamond cylinder; the diamond films deposited and grown on the upper surface and the lower surface of the substrate are connected into a whole through the diamond cylinders in the through holes.
Preferably, the diameter of the through hole is larger than 0.1 mm; the diamond film does not completely fill the through hole to form a hollow diamond tube body; the diamond films deposited and grown on the upper surface and the lower surface of the substrate are connected into a whole through the diamond tube body on the inner wall of the through hole.
Preferably, the number of the through holes is multiple, and the distance between the through holes is larger than the diameter of the through holes.
As a preferred solution, the thermal expansion coefficient of the substrate used is matched to that of diamond; the substrate is a composite sheet formed by one or more of a silicon wafer, silicon nitride, silicon carbide, aluminum oxide, an aluminum nitride ceramic sheet, steatite porcelain, a microcrystalline glass sheet, a graphite sheet or a carbon fiber sheet.
Preferably, the diamond film is a polycrystalline diamond film.
Preferably, the thickness of the diamond film is less than 200 microns.
The manufacturing method for preparing the diamond compact with the communicating holes comprises the following steps:
s10, manufacturing through holes penetrating through the upper surface and the lower surface of the substrate to form a substrate with holes;
s20, respectively depositing and growing diamond films on the upper surface, the lower surface and the through holes of the substrate with the holes to obtain the diamond composite sheet.
Preferably, the method further comprises the following steps between step S10 and step S20: and cleaning the substrate with the holes, polishing the upper surface and the lower surface of the substrate with the holes, and cleaning the polished substrate with the holes for the second time.
As a preferable scheme, the step S20 includes the steps of:
s21, depositing and growing a diamond film on the upper surface of the substrate with the holes, and taking out the diamond film when the diamond film on the upper surface grows to a certain thickness;
s22, after carbon deposition is cleaned on the lower surface of the substrate with the holes, a diamond film is deposited on the lower surface, and the diamond film is taken out after the diamond film on the lower surface grows to a certain thickness;
s23, after carbon deposition is cleaned on the upper surface of the substrate with the hole, a diamond film is deposited on the upper surface, and the diamond film is taken out when the diamond film on the upper surface grows to a certain thickness;
and (5) continuously repeating the step (S22) and the step (S23), and alternately growing the two surfaces for multiple times until the thicknesses of the diamond film layers on the upper surface and the lower surface of the substrate and the inner wall of the through hole reach the required thickness to obtain the diamond compact.
The invention has the beneficial effects that:
because the diamond has various excellent performances such as high thermal conductivity, high insulation resistance, low dielectric constant, high hardness, high chemical stability and the like, after the diamond is combined with a substrate, the insulation resistance and the environmental weather resistance of the substrate can be obviously improved, and the dielectric constant is reduced;
in addition, the substrate is prepared into a structure with holes, the diamond films are also grown in the through holes, and the diamond films on the upper surface and the lower surface are connected together by the diamond in the through holes, so that a high-speed channel is formed between the upper surface and the lower surface of the substrate by heat, and the effect of increasing the heat conductivity is obvious; the through holes can also improve the thermal stability and the film adhesion of the composite sheet;
finally, the composite sheet of the present invention has significant cost advantages over the use of pure self-supporting polycrystalline diamond sheets.
Drawings
Fig. 1 is a schematic structural view of a first embodiment of a diamond compact with interconnected pores according to the present invention.
Fig. 2 is a schematic structural view of a second embodiment of the diamond compact with interconnected pores of the present invention.
Fig. 3 is a block flow diagram of a method of manufacturing a diamond compact with interconnected pores according to the present invention.
The reference numbers indicate: 1. 1 a-a substrate; 2. 2 a-diamond film; 3. 3 a-a via; 4-a diamond cylinder; 5-diamond tube body.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
Referring to fig. 1, the present invention relates to a diamond compact with communication holes, comprising a substrate 1, wherein the substrate 1 is provided with at least one through hole 3 penetrating through the upper surface and the lower surface thereof; the diamond composite sheet with the communicating holes 3 also comprises a diamond film 2, and the diamond film 2 is deposited and grown on the upper surface and the lower surface of the substrate 1 and the inner wall of the through holes 3. Because the diamond has various excellent performances such as high thermal conductivity, high insulation resistance, low dielectric constant, high hardness, high chemical stability and the like, after the diamond is combined with the substrate 1, the insulation resistance and the environmental weatherability of the substrate 1 can be obviously improved, and the dielectric constant is reduced; the substrate 1 is prepared into a structure with holes, the diamond films 2 are also grown in the through holes 3, and the diamond films 2 on the upper surface and the lower surface of the substrate 1 are connected together by the diamond in the through holes 3, so that a high-speed channel is formed between the upper surface and the lower surface of the substrate 1 by heat, and the effect of increasing the heat conductivity is obvious; the through holes 3 can also improve the thermal stability and the film adhesion of the composite sheet; compared with the pure self-supporting polycrystalline diamond sheet, the composite sheet has obvious cost advantage.
In addition, the thickness of the diamond film 2 is less than 200 mm, preferably the polycrystalline diamond film 2 with the thickness of 100 microns, the through holes 3 are multiple and are arranged in an array, the distance between the through holes 3 is larger than the diameter of the through holes 3, and the preferred hole distance is 1 mm; and the diameter of the through hole 3 is less than 0.4 mm, the diamond film 2 completely fills the through hole 3 to form a diamond column 4, and the diamond column 4 is connected with the diamond film 2 deposited and grown on the upper surface and the lower surface of the substrate 1 into a whole.
The thermal expansion coefficient of the used substrate 1 is matched with that of diamond, and the thermal expansion coefficients of the substrate and the diamond are close; specifically, the substrate 1 is a composite sheet formed by combining one or more of a silicon wafer, silicon nitride, silicon carbide, aluminum oxide, an aluminum nitride ceramic sheet, steatite porcelain, a microcrystalline glass sheet, a graphite sheet or a carbon fiber sheet; the substrate 1 is preferably a carbon fiber sheet.
As shown in fig. 2, a second embodiment of the diamond compact with interconnected pores according to the present invention is different from the first embodiment in that the diameter of the through hole 3a is larger than 0.1 mm, and the diamond film 2a does not completely fill the through hole 3a to form a hollow diamond tube 5, and the diamond tube 5 is integrally connected with the diamond films 2a deposited and grown on the upper and lower surfaces of the substrate 1 a.
Whether the diamond tube body 5 or the diamond column body 4 is adopted, the diamond films 2 and 2a on the upper surface and the lower surface are connected together through the through holes 3 and 3a, so that a high-speed channel is formed between the upper surface and the lower surface of the substrates 1 and 1a by heat, and the effect of increasing the heat conductivity is obvious; and the through holes 3 and 3a can also improve the thermal stability and the film adhesion of the composite sheet.
Referring to fig. 3, the present invention relates to a method for manufacturing a diamond compact with interconnected pores, comprising the following steps:
s10, manufacturing through holes penetrating through the upper surface and the lower surface of the substrate to form a substrate with holes;
and S20, respectively depositing and growing diamond films on the upper surface and the lower surface of the substrate with the holes and in the through holes of the substrate with the holes to obtain the diamond composite sheet.
The method has simple steps, and the diamond compact prepared by the method has the properties of high hardness, high thermal conductivity, high insulation resistance, low dielectric constant, high chemical stability and the like, and has obvious cost advantage compared with a pure self-supporting polycrystalline diamond sheet.
In addition, the following steps are also included between step S10 and step S20: cleaning the substrate with the holes, polishing the upper surface and the lower surface of the substrate with the holes, and then cleaning the polished substrate with the holes for the second time, wherein the cleaning for the second time is ultrasonic cleaning.
Specifically, the second step comprises the following steps:
s21, depositing and growing a diamond film on the upper surface of the substrate with the holes, and taking out the diamond film when the diamond film on the upper surface grows to a certain thickness;
s22, after carbon deposition is cleaned on the lower surface of the substrate with the holes, a diamond film is deposited on the lower surface, and the diamond film is taken out after the diamond film on the lower surface grows to a certain thickness;
s23, after carbon deposition is cleaned on the upper surface of the substrate with the holes, depositing a diamond film on the upper surface, and taking out the diamond film when the diamond film on the upper surface grows to a certain thickness;
and (5) continuously repeating the step (S22) and the step (S23), and alternately growing the two surfaces for multiple times until the thicknesses of the diamond film layers on the upper surface and the lower surface of the substrate and the inner wall of the through hole reach the required thickness to obtain the diamond compact.
According to the above steps of the manufacturing method, the present invention herein provides the following two preferred embodiments.
Example one
Firstly, processing an array type communication hole on a carbon fiber sheet by using laser equipment, wherein the diameter of the communication hole is 0.2 mm, and the pitch of the holes is 1 mm; cleaning the carbon fiber sheet, polishing the upper surface and the lower surface of the carbon fiber sheet by using a 2000-mesh diamond grinding wheel, and putting the polished carbon fiber sheet into a dispersion liquid containing 400-mesh diamond micropowder for ultrasonic cleaning; putting the polished and ultrasonically cleaned carbon fiber sheet with the communicating hole into a microwave plasma enhanced chemical vapor deposition system (MPCVD) to start to deposit and grow a polycrystalline diamond film, firstly, performing deposition growth on the upper surface of the carbon fiber sheet, and taking out the carbon fiber sheet when the diamond film layer on the upper surface grows to 10 microns; after carbon on the lower surface of the carbon fiber sheet is cleaned, the lower surface of the carbon fiber sheet is placed upwards into a microwave plasma enhanced chemical vapor deposition system to continue to grow a polycrystalline diamond film, the steps can be repeated in order to reduce the bending of the composite sheet under the action of stress, and the two surfaces of the carbon fiber sheet alternately grow for multiple times until the diamond films on the upper surface and the lower surface of the carbon fiber sheet and in the through hole reach 100 micrometers, and then the growth is stopped.
Example two
Firstly, processing an array type communicating hole on an aluminum nitride ceramic wafer by using laser equipment, wherein the diameter of the through hole is 0.2 mm, and the pitch of the holes is 2.5 mm; cleaning the aluminum nitride ceramic wafer, polishing the upper surface and the lower surface of the aluminum nitride ceramic wafer by using a 2000-mesh diamond grinding wheel, and putting the polished aluminum nitride ceramic wafer into a dispersion liquid containing 400-mesh diamond micro powder for ultrasonic cleaning; putting the polished and ultrasonically cleaned aluminum nitride ceramic wafer with the communicating hole into a microwave plasma enhanced chemical vapor deposition system (MPCVD) to start to deposit and grow a polycrystalline diamond film, firstly, performing deposition growth on the upper surface of the aluminum nitride ceramic wafer, and taking out the aluminum nitride ceramic wafer when the diamond film layer on the upper surface grows to 10 microns; after carbon deposition on the lower surface of the aluminum nitride ceramic wafer is cleaned, the lower surface of the aluminum nitride ceramic wafer is placed upwards into a microwave plasma enhanced chemical vapor deposition system to continue to grow the polycrystalline diamond film, in order to reduce the bending of the composite sheet under the action of stress, the steps can be repeated, the two surfaces alternately grow for multiple times, and the growth is stopped until the diamond films on the upper surface, the lower surface and the through hole of the aluminum nitride ceramic wafer reach 100 micrometers.
In both examples, the purpose of diamond grinding and ultrasonic cleaning of the dispersion of diamond micropowder is to enhance the nucleation density and adhesion of the diamond in subsequent processing steps.
The above embodiments are merely illustrative of the preferred embodiments of the present invention, and not restrictive, and various changes and modifications to the technical solutions of the present invention may be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are intended to fall within the scope of the present invention defined by the appended claims.

Claims (8)

1. A diamond compact with communication holes comprises a substrate and is characterized in that: the substrate is provided with at least one through hole penetrating through the upper surface and the lower surface of the substrate; the diamond composite sheet with the communicating hole also comprises a diamond film, and the diamond film fills the through hole; the diamond film is deposited and grown on the upper surface and the lower surface of the substrate and the inner wall of the through hole of the substrate;
the manufacturing method of the diamond compact with the communicating hole comprises the following steps:
s10, manufacturing through holes penetrating through the upper surface and the lower surface of the substrate to form a substrate with holes;
s20, respectively depositing and growing diamond films on the upper surface and the lower surface of the substrate with the holes and in the through holes of the substrate with the holes to obtain the diamond composite sheet, which specifically comprises the following steps:
s21, depositing a diamond film on the upper surface of the substrate with the hole, and taking out the substrate when the diamond film on the upper surface grows to a certain thickness;
s22, after carbon deposition is cleaned on the lower surface of the substrate with the holes, a diamond film is deposited on the lower surface, and the diamond film is taken out after the diamond film on the lower surface grows to a certain thickness;
s23, after carbon deposition is cleaned on the upper surface of the substrate with the holes, depositing a diamond film on the upper surface, and taking out the diamond film when the diamond film on the upper surface grows to a certain thickness;
and (5) continuously repeating the step (S22) and the step (S23), and alternately growing the two surfaces for multiple times until the thicknesses of the diamond film layers on the upper surface and the lower surface of the substrate and the inner wall of the through hole reach the required thickness to obtain the diamond compact.
2. The diamond compact with interconnected pores of claim 1, wherein: the diameter of the through hole is less than 0.4 mm; the diamond film completely fills the through hole to form a diamond cylinder; the diamond films deposited and grown on the upper surface and the lower surface of the substrate are connected into a whole through the diamond cylinders in the through holes.
3. The diamond compact with interconnected pores of claim 1, wherein: the diameter of the through hole is larger than 0.1 mm; the diamond film does not completely fill the through hole to form a hollow diamond tube body; the diamond films deposited and grown on the upper surface and the lower surface of the substrate are connected into a whole through the diamond tube body on the inner wall of the through hole.
4. The diamond compact with interconnected pores of claim 1, wherein: the through holes are multiple in number, and the distance between the through holes is larger than the diameter of the through holes.
5. The diamond compact with interconnected pores of claim 1, wherein: the thermal expansion coefficient of the used substrate is matched with that of the diamond; the substrate is a composite sheet formed by one or more of a silicon wafer, silicon nitride, silicon carbide, aluminum oxide, an aluminum nitride ceramic sheet, steatite porcelain, a microcrystalline glass sheet, a graphite sheet or a carbon fiber sheet.
6. The diamond compact with interconnected pores of claim 1, wherein: the diamond film is a polycrystalline diamond film.
7. The diamond compact with interconnected pores of claim 1, wherein: the thickness of the diamond film is less than 200 microns.
8. The diamond compact with interconnected pores of claim 1, further comprising the following steps between step S10 and step S20: and cleaning the substrate with the holes, polishing the upper surface and the lower surface of the substrate with the holes, and cleaning the polished substrate with the holes for the second time.
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