CN114324458B - Interface thermal conductivity test sample and method of forming the same - Google Patents
Interface thermal conductivity test sample and method of forming the same Download PDFInfo
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- CN114324458B CN114324458B CN202111618128.0A CN202111618128A CN114324458B CN 114324458 B CN114324458 B CN 114324458B CN 202111618128 A CN202111618128 A CN 202111618128A CN 114324458 B CN114324458 B CN 114324458B
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Abstract
The application discloses a pretreatment method for a material to be detected, which comprises the steps of obtaining a sheet sample, taking one side surface of the sheet sample perpendicular to the thickness direction as a target surface, wherein reinforcing phase particles are arranged in the sheet sample; selecting the exposed reinforcing phase particles in the target surface as target particles, wherein the exposed surface of the target particles is used as a reference surface; placing the sheet sample in a sample inserting groove, and adjusting the included angle between the target surface and the groove bottom to be a preset inclination angle; injecting a mounting colloid into the mounting groove and solidifying to obtain a mounting sample wrapped with the sheet sample; and polishing the embedded sample along the direction of the target particles on one side surface of the embedded sample until the distance between the polishing surface and the edge of the reference surface of the target particles is smaller than or equal to a preset distance, so as to obtain a test sample, wherein the polishing surface is used as the tested surface of the test sample. The above method enables the preparation of test samples satisfying TDTR test.
Description
Technical Field
The application relates to the technical field of thermal conductivity testing, in particular to an interface thermal conductivity testing sample and a forming method thereof.
Background
With the rapid development of the electronic information manufacturing industry, the integration level requirement of the electronic chip is higher and the feature size requirement is smaller, so that the heat dissipation problem of the electronic device is more serious, the current heat dissipation mechanism cannot meet the increasing heat dissipation requirement, and therefore, the problem of how to develop a heat dissipation material which has high heat conductivity coefficient and thermal expansion coefficient and is matched with a semiconductor material is needed to be solved. Many researchers at home and abroad develop researches on the high-heat-conductivity metal matrix composite material, wherein the high-heat-conductivity metal matrix composite material has the characteristic of high heat conductivity, and the thermal expansion coefficient is matched with that of a semiconductor material, so that the high-heat-conductivity metal matrix composite material has great potential and application prospect in solving the heat dissipation problem of electronic devices.
In the process of optimizing the heat conduction performance of the high-heat-conduction metal-based composite material, the interface plays an extremely important role in the heat conduction performance of the composite material, so that the optimization of the heat conduction performance of the interface between the metal matrix and the enhanced phase is one of the current research hot spots. The technical problem of interfacial thermal conductivity measurement must be solved in researching the interfacial thermal conductivity of the metal matrix composite, and the time domain thermal reflection measurement method (TDTR) developed in recent years can be used for measuring the interfacial thermal conductivity of the nano-scale composite, thus providing a technical foundation for the thermal conductivity research of the metal matrix composite. However, because the strength difference between the matrix and the reinforcing phase in the metal matrix composite material is large, the granularity of the reinforcing phase is small, the appearance is complex, and the sample for TDTR testing which meets the requirements in the prior art is difficult to grind and polish, so that the accurate measurement of the interfacial thermal conductivity of the composite material is difficult.
Disclosure of Invention
In view of the above, the present application provides an interface thermal conductivity test sample and a method for forming the same, so as to solve the problem that the existing composite material interface with a particle reinforced phase is difficult to accurately measure.
The application provides a method for forming an interface thermal conductivity test sample, which comprises the following steps: pretreating a material to be detected to obtain a sheet sample, wherein a surface of one side of the sheet sample perpendicular to the thickness direction is used as a target surface, and reinforcing phase particles are arranged in the sheet sample; selecting the exposed reinforcing phase particles in the target surface as target particles, wherein the exposed surface of the target particles is used as a reference surface; placing the sheet sample in a sample inserting groove, and adjusting the included angle between the target surface and the groove bottom to be a preset inclination angle; injecting a mounting colloid into the mounting groove and solidifying to obtain a mounting sample wrapped with the sheet sample; and polishing the embedded sample along the direction of the target particles on one side surface of the embedded sample until the distance between the polishing surface and the edge of the reference surface of the target particles is smaller than or equal to a preset distance, so as to obtain a test sample, wherein the polishing surface is used as the tested surface of the test sample.
Optionally, the method further comprises: and forming a reflecting layer on the polished surface.
Optionally, taking a side surface of the target particle, which is positioned in the sheet-shaped sample and is adjacent to the reference surface, as a test surface of the target particle; and performing polishing along the surface of the embedded sample opposite to the test surface in the direction of the test surface.
Optionally, an included angle α is formed between the reference surface and the test surface, the preset inclination angle is β, a target included angle between the reference surface and the polishing surface of the test sample is θ, and the preset inclination angle is determined according to the following relationship: beta=180 ° -alpha-theta.
Optionally, the test sample is for TDTR tests; the maximum value theta max of the target included angle meets the following conditions: θ is less than or equal to θ max,θmax =arctan (r/H), where r is the spot radius of the laser used in TDTR test, and H is the peak-to-trough amplitude of the topography relief of the measured surface.
Optionally, the roughness of the measured surface is less than or equal to 60nm, the amplitude H ranges from 200nm to 250nm, the light spot radius r ranges from 5 μm to 40 μm, and the target included angle theta ranges from 0 DEG to 5 deg.
Optionally, the preset distance is in a range of 0-200 nm.
Optionally, the polishing adopts more than two grinding wheels from thick to thin, and sequentially polishes the embedded sample; the mesh number of the selected grinding wheels is 300-200 meshes, and the grinding and polishing rotating speed is 100-250 rpm.
Optionally, the step of injecting the plate-inserting colloid into the plate-inserting groove and curing is performed under normal pressure.
The application also provides an interface thermal conductivity test sample, comprising: the surface of one side of the solidified colloid is covered with a reflecting layer, and the surface of the reflecting layer is used as a surface to be measured; a sheet sample within the cured gel, the sheet sample having target particles therein; the target particles have a reference surface and a test surface, the reference surface being exposed to one side surface of the sheet-like sample; the test surface is adjacent to the reference surface, the test surface faces the surface to be tested, and an included angle between the test surface and the surface to be tested is a target included angle, and the target included angle is more than or equal to 0.
Optionally, the test sample is for TDTR tests; the maximum value theta max of the target included angle meets the following conditions: θ is less than or equal to θ max,θmax =arctan (r/H), where r is the spot radius of the laser used in TDTR test, and H is the peak-to-trough amplitude of the topography fluctuation of the measured surface.
Optionally, the roughness of the measured surface is less than or equal to 60nm, the amplitude H ranges from 200 nm to 250nm, the light spot radius r ranges from 5 μm to 40 μm, and the target included angle theta ranges from 0 DEG to 5 deg.
The application also provides an interface thermal conductivity test sample formed by the forming method of any one of the above.
Aiming at the requirement of TDTR on measuring the sample by interface thermal conductivity, the small-angle inclined polishing technology adopted by the invention can obtain the test sample with the interface size, the interface size and the interface roughness meeting the requirements, realizes the measurement of the metal matrix composite interface thermal conductivity, and provides a rapid polishing technology for sample preparation meeting TDTR test for the research of block sample interface thermal conductivity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic illustration of a film sample according to one embodiment of the present application being tested TDTR;
FIG. 2 is a schematic structural view of a metal matrix composite;
FIG. 3 is a flow chart of a method of forming a test sample according to an embodiment of the application;
FIG. 4 is a partial schematic view of the test sample formed in accordance with an embodiment of the present application;
Fig. 5 to 9 are schematic structural views illustrating a process of forming a test sample according to an embodiment of the present application.
Detailed Description
As described in the background, the prior Time Domain Thermal Reflectometry (TDTR) is subject to stringent sample requirements. As shown in fig. 1, time Domain Thermal Reflection (TDTR) requires a high thermal reflectivity of the sample surface, so the roughness of the light reflecting layer of the sample surface is usually small; the thermal penetration depth of the time domain thermal reflectometry method can reach 300nm at the highest, so that the composite two-phase interface of the composite material sample, namely the vertical distance (namely the normal dimension of the interface) between the interface of the particle reinforced phase and the metal matrix in the figure 1 and the surface of the sample is required to be in the range of 0-300 nm; the transverse dimension (namely the lateral dimension of the interface) of the composite two-phase interface of the composite material sample is larger than the dimension of the light spot of the emitted laser, the light spot of the time domain heat reflection method is usually a circular light spot, and the radius is usually 5-40 microns; this presents challenges for interface thermal conductivity testing and sampling of metal matrix composites.
Because the size and thickness of the interface between the reinforced phase and the metal matrix of the metal matrix composite are not uniform and controllable, it is difficult to obtain a sample with the size and thickness meeting the requirements of the interface thermal conductivity test through simple grinding and polishing, for the metal matrix composite with larger strength difference between the particle reinforced phase and the metal matrix, the reinforced phase is dispersed and distributed in the metal matrix, and the interface shape is complex because of smaller interface size between the dispersed phase and the metal matrix, as shown in fig. 2, wherein (1) is a perspective schematic diagram, and (2) is a cross-section schematic diagram. It is difficult to obtain an interface thermal conductivity test sample with interface dimensions, interface roughness and interface thickness all meeting test requirements by a conventional polishing means.
At present, a layered metal matrix composite film can be prepared by adopting a vacuum evaporation method to obtain a two-phase composite interface of the composite material. The laminar film sample itself already meets the interface size required by TDTR test, the thickness of two phases can be regulated and controlled by regulating and controlling the sample preparation process, and the roughness requirement is met by optimizing the polishing process, such as single-sided polishing and polishing processes which are parallel to the film direction and are performed on the composite laminar film sample by adopting planetary polishing equipment, so that the sample can meet the requirement of TDTR test. Therefore, the object and the focus of the current preparation method of the time domain thermal reflection method sample are mainly to reduce the surface roughness of the film sample, and although the interface thermal conductivity test can be performed on most of the thermal conductive films, the interface thermal conductivity test requirement of the metal matrix composite block material cannot be met. Because the interface thermal conductance of the layered composite film and the composite block sample always has a certain difference, it is very necessary to find a metal-based composite block material sample preparation method meeting the TDTR interface thermal conductance test requirement.
Aiming at the requirement of TDTR on measuring the sample by interface thermal conductivity, the small-angle inclined polishing technology adopted by the invention can obtain the sample with the interface size, the interface size and the interface roughness meeting the requirement, realize the measurement of the interface thermal conductivity of the metal matrix composite, provide a rapid polishing technology for sample preparation meeting TDTR test for the research of block sample interface thermal conductivity, and solve the problem of sample preparation of the metal matrix composite.
The following description of the embodiments of the present application will be made in detail and with reference to the accompanying drawings, wherein it is apparent that the embodiments described are only some, but not all embodiments of the present application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to fall within the scope of the application. The various embodiments described below and their technical features can be combined with each other without conflict.
Fig. 3 is a flow chart illustrating a method for forming an interface thermal conductivity test sample according to an embodiment of the invention.
The forming method comprises the following steps:
Step S101, preprocessing a material to be detected to obtain a sheet sample, wherein one side surface of the sheet sample perpendicular to the thickness direction is used as a target surface, and reinforcing phase particles are arranged in the sheet sample.
The pretreatment may include a wire-cut process to cut the composite material (block) into sheet-like samples, such as round sheets. The composite material is a metal matrix doped with reinforcing phase particles. To ensure that sufficient reinforcing phase particles are exposed at the surface of the metal matrix block, the target surface size (maximum length) of the cut sheet sample should be greater than 5mm. Preferably, the sheet sample is disc-shaped, and the diameter is greater than 5mm.
In order to facilitate subsequent grinding and polishing to obtain complete particle reinforced phase inclined planes with specific angles, the thickness of the sheet sample is greater than 1mm, so that the sheet sample at least contains finished reinforced phase particles. After the cutting is completed, the surface of the sheet sample is cleaned and dried, and rough grinding can be performed to a certain degree to reduce the roughness.
Step S102: and selecting the exposed reinforcing phase particles in the target surface as target particles, wherein the exposed surface of the target particles is used as a reference surface.
The surface morphology of the sheet sample can be observed by a high-resolution optical microscope, the particle size is selected to be proper according to the requirement that the particle size is required to be larger than the spot size of laser light tested by TDTR, and reinforcing phase particles with the particle surfaces parallel to the target surface are marked nearby.
Since the randomly distributed reinforcing phase particles are present in the composite material, the cut surface always exposes the surface of at least one reinforcing phase particle by a wire-cut process. One of the particles is selected as the target particle according to the size of the exposed particle surface, which serves as the reference surface. Since TDTR tests employ laser spot radii typically ranging from 5 to 40 μm, particles with an exposed surface size (maximum length) of at least 40 μm (length in each direction) were selected as target particles. In some embodiments, the exposed surface has a dimension greater than 60 μm. The reference surface is determined to determine a test surface for a subsequent test.
Step S103: and placing the sheet sample in a sample inserting groove, and adjusting the included angle between the target surface and the groove bottom to be a preset inclination angle.
Since the reinforcing phase having a high hardness mostly has a stable crystal structure and a specific crystal plane orientation, the reinforcing phase mostly has a regular shape, and the reinforcing phase is usually particles of a substance having a high hardness, such as diamond, silicon carbide, titanium carbide, tungsten carbide, etc., and generally has a stable crystal structure and a specific crystal plane orientation, and therefore the reinforcing phase mostly has a regular shape, such as regular octahedron, regular dodecahedron, cubo-octahedron, hexagonal crystal, etc. After the reference surface of the target particle is determined, although other surfaces are located within the substrate, the relative positions of the other surfaces can be substantially determined after the reference surface is determined, knowing the particulate matter.
Further, a side surface of the target particle, which is positioned in the sheet-like sample and is adjacent to the reference surface, is used as a test surface of the target particle. An included angle alpha is formed between the reference surface and the test surface, and the included angle alpha is determined by the grain shape of the particles.
The inclination angle between the sheet sample and the bottom of the mounting groove can be realized by providing a supporting column with a certain height below the sheet sample and adjusting the position of the sheet sample.
Step S104: and injecting a sample-inserting colloid into the sample-inserting groove and solidifying to obtain the embedded sample wrapped with the sheet sample.
The mounting colloid can be resin and the like, can be solidified without applying pressure, and the hardness after solidification meets the requirement of not deforming during polishing. The bezel colloid floods the sheet sample.
In this embodiment, the mounting colloid is a bi-component mixed normal temperature solidified epoxy resin fluid, and after mixing, the temperature is raised automatically, and after cooling to normal temperature, the sample to be mounted with the sheet sample is obtained.
Step S105: and polishing the embedded sample along the direction of the target particles on one side surface of the embedded sample until the distance between the polishing surface and the edge of the reference surface of the target particles is smaller than or equal to a preset distance, so as to obtain a test sample, wherein the polishing surface is used as the tested surface of the test sample.
The embedded sample can be polished by an automatic polishing machine, and in the polishing process, more than two polishing wheels from thick to thin can be adopted to sequentially polish the embedded sample. The grinding wheels with different diameters with the mesh number ranging from 300 meshes to 2000 meshes can be selected. Preferably, the polishing rotation speed range can be set to be 100-250 rpm, so that the polishing efficiency is improved while the polishing effect is ensured.
Preferably, the polishing may be performed along a surface of the inlay sample opposite to the test surface, and in a direction toward the test surface, and may be rapidly polished to a proper position. Because TDTR tests have requirements on the longitudinal depth and the transverse dimension of the interface, if polishing and grinding are excessive, the test surface is polished, so that the transverse dimension of the interface is reduced, and the TDTR test requirements cannot be met; if the polishing stop position is too large from the edge position of the reference surface, the longitudinal depth between the test surface and the tested surface of the sample is too large and exceeds the laser heat penetration depth. Since a reflective layer of about 80nm is formed on the polishing surface, and the laser thermal penetration depth is typically about 300nm, it is preferable that the predetermined distance between the polishing stop position and the edge of the reference surface is in the range of 0 to 200 μm. In other embodiments, a reasonable preset distance may be set according to the specific situation.
When the reinforced phase of the metal matrix composite is in a regular shape, a sample preparation technology of small-angle inclined polishing is adopted, and a measurable interface of the particle reinforced phase and the metal matrix can be obtained. In the polishing process, because the hardness of the particles is high and the particles are difficult to grind, the polishing process can only take away the metal on the surface or independent particles, and finally reinforcing phase particles are distributed on the surface of a polishing sample.
A light reflecting layer, such as an aluminum layer, may also be formed on the polished surface.
Fig. 4 is a schematic diagram of a portion of the test sample according to an embodiment of the invention.
In the finally formed test sample, the target particles are metal layers with certain thickness, the certain metal layer thickness h corresponds to a certain target included angle theta, and when the transverse dimension of the test surface of the reinforced phase particles is L, theta=arctan (h/L).
In some embodiments, in step S103, the preset inclination angle β between the target surface of the sheet sample and the groove bottom may be determined according to the following relationship: beta=180 ° -alpha-theta. Alpha is the included angle between the reference surface and the test surface of the target particle.
Preferably, the target included angle θ is equal to an undulating angle of the light reflecting layer. When used in TDTR test, to meet TDTR test requirements, the maximum value θ max of the target included angle θ (i.e., the maximum relief angle of the light reflecting layer) meets: and θ max＝arctan(r/H),θ≤θmax,, wherein r is the spot radius of laser adopted in TDTR test, and H is the peak-to-trough amplitude of the topography fluctuation of the measured surface. Wherein, the smaller θ, the more the metal layer is parallel to the inclined plane of the reinforcing phase particles, the more similar the interface morphology is to the film sample.
In some embodiments, TDTR test requires that the roughness of the surface being measured be less than or equal to 60nm, which is the root mean square or arithmetic average of the relief height at each location of the surface being measured. Under the condition that the maximum roughness is 60nm, the amplitude range H from the crest to the trough of the topography fluctuation of the measured surface is 200-250 nm, and when the laser is adopted, the light spot radius r range is 5-40 mu m, the laser can be used for measuring the surface by: θ max =arctan (r/H), calculated as θ max =5°. The target included angle theta ranges from 0 degrees to 5 degrees.
Fig. 5 to 9 are schematic structural diagrams illustrating a process of forming a test sample according to an embodiment of the invention.
In this example, the formation of a test sample of the present invention is illustrated using a copper/diamond composite bulk material as an example. Wherein the diamond reinforcing phase particles are regular octahedrons with dihedral angles (included angles between adjacent surfaces on two sides of the same edge) of 109 degrees, and the particle size is in the range of 60-100 mu m.
(1) Cutting: the metal matrix composite block material was wire cut to obtain standard wafers 100 (see fig. 5) having a size smaller than the size of the cold mosaic mold, a diameter of about 5-20mm and a height of about 5-10mm. And cleaning and drying the surface of the standard wafer of the metal matrix composite.
(2) Observing the surface morphology: the surface morphology of the metal matrix composite wafer is observed by means of a light mirror, diamond particles with a particle size of more than 60 μm and a particle surface parallel to the wafer surface are selected as target particles 101, and marks are made in the vicinity thereof. The exposed surface of the target particle 101 is a reference surface 1011, and a surface adjacent to the reference surface 1011 is a test surface 1012 (see fig. 5).
(3) Tilting mounting: referring to fig. 6, the standard wafer 100 is obliquely put into a mold 200 (refer to fig. 6), and since the dihedral angle of the regular octahedron is 109 °, the position of the standard wafer 100 relative to the supporting resin 201 is adjusted so that the included angle β between the target surface and the bottom surface of the mold 200 is 66 ° to 71 °, and then the two-component mixed normal temperature curing epoxy resin 202 is poured into and cured to obtain the inlay sample 300. The inlay sample 300 was taken out of the mold, and the inlay operation was completed, resulting in an inlay sample 300 as shown in fig. 7. To facilitate adjustment of the tilt angle, in this embodiment, the target surface of the wafer 100 is placed toward the bottom of the mold 200, and in other embodiments, the target surface may be placed upward. The included angle β may be adjusted by adjusting the height of the support value 201, the position of the support resin 201, and the position of the wafer 100.
The TDTR test in the prior art usually adopts a hot-inlaid method for inlaying, and the hot-inlaid method is usually carried out at high temperature (about 180 ℃) and high pressure (about 250 bar), so that the pressure is exerted from top to bottom, the inclination angle of the obliquely arranged sheet sample can be influenced, and the sample with the accurately controlled angle cannot be prepared. Therefore, the invention adopts a cold inlaying method, the inclination angle of the sheet sample is adjusted well, then the sheet sample and the supporting resin are poured into the mixed epoxy resin fluid, the sheet sample and the supporting resin are immersed into the mixed epoxy resin fluid, the mixture is cooled to room temperature after self-heating, and then solidified, no extra pressure is required to be applied, and the inclination angle of the sheet sample is not influenced, so that the sample with the accurate control of the inclination angle can be obtained.
(4) Grinding and polishing by a grinding and polishing machine: the embedded sample 300 is polished by an automatic polishing machine, along the opposite surface of the test surface 1012, towards the test surface 1012. In the grinding and polishing process, the grinding wheels are replaced according to the sequence of 320 meshes, 600 meshes and 1200 meshes; the rotating speed of the grinding disc is 100-250rpm; and (3) polishing time is 60s, and finally a polished sample with interface roughness less than 30nm is obtained, wherein a schematic cross section of the polished sample is shown in fig. 8.
(5) Plating Al on the surface: the surface of the polished sample is cleaned, an Al thin layer 400 with the thickness of about 80nm is evaporated on the inclined surface of the sample by adopting a vacuum evaporation method to serve as a heat reflection layer, the interface roughness after Al plating is less than 60nm, TDTR testing is facilitated, and an obtained sample schematic diagram is shown in fig. 9.
(6) And cleaning and drying, carrying out TDTR heat conduction test on the obtained metal matrix composite sample in the illustrated area, and carrying out fitting calculation on the obtained TDTR test data to obtain the interface heat conduction value of the metal matrix composite block material.
When TDTR is carried out, the test parameters are consistent with those of the film sample in the prior art, and the thickness of the heat reflection layers plated on the block sample and the film sample is consistent and is about 80 nm; TDTR the test frequency was 50KHz and the spot size was 40 μm. Under the same parameter setting, the interfacial thermal conductivity value obtained by carrying out TDTR test is not much different from 68+/-4 MW/(m 2.K) obtained by adopting a film sample. Therefore, the metal matrix block composite sample prepared by the small-angle inclined polishing technology can be considered to meet the requirement of TDTR test, and can be used for testing the interface thermal conductivity of a metal matrix and an enhancement phase.
Aiming at the requirement of TDTR on measuring the sample by interface thermal conductivity, the small-angle inclined polishing technology adopted by the invention can obtain the test sample with the interface size, the interface size and the interface roughness meeting the requirements, realizes the measurement of the metal matrix composite interface thermal conductivity, and provides a rapid polishing technology for sample preparation meeting TDTR test for the research of block sample interface thermal conductivity.
The embodiment of the application also provides an interface thermal conductivity test sample.
Fig. 8 is a schematic structural diagram of a test sample according to an embodiment of the application.
In this embodiment, the test sample includes a cured gel 500, where a surface of one side of the cured gel 500 is covered with a reflective layer 400, and a surface of the reflective layer 400 is used as a surface to be tested; a sheet-like sample 100 located within the solidified colloid 500, the sheet-like sample 100 having target particles 101 therein; the target particle 101 has a reference surface 1011 and a test surface 1012, the reference surface 1011 being exposed to a side surface of the sheet-like sample 100; the test surface 1012 is adjacent to the reference surface 1011, and the test surface 1012 faces the surface to be tested, and an included angle between the test surface 1012 and the surface to be tested is a target included angle θ, where the target included angle θ is greater than or equal to 0.
The sheet sample 100 may be a metal matrix doped with reinforcing phase particles, such as a copper matrix doped with diamond particles. In fig. 9, only the target particles 101 therein are shown. The sheet sample 100 may be circular with a diameter greater than 5mm; the thickness should be greater than 1mm. The reference surface has a dimension greater than 40 μm, preferably greater than 60 μm.
The test sample is used for TDTR tests; the maximum value theta max of the target included angle meets the following conditions: θ is less than or equal to θ max,θmax =arctan (r/H), where r is the spot radius of the laser used in TDTR test, and H is the peak-to-trough amplitude of the topography fluctuation of the measured surface.
In some embodiments, the roughness of the measured surface of the test sample is less than or equal to 60nm, the amplitude H ranges from 200nm to 250nm, the spot radius r ranges from 5 μm to 40 μm, and the target included angle θ ranges from 0 ° to 5 °.
The test sample may be formed by the formation method in the previous embodiment.
The main innovation point of the test sample and the forming method thereof is that the technology of small-angle inclined grinding and polishing sample preparation is adopted, so that an interface between the metal matrix and the reinforced phase particles, which meets the TDTR test requirement, is obtained, namely, the interface roughness is small enough, the interface size is larger than the size of a detection light spot, the interface thickness is within the thermal penetration depth of TDTR method, and a technical foundation is provided for the research of the heat conducting property of the metal matrix composite material. Mainly solves the technical problems in the following four aspects: (1) Rapidly polishing the metal matrix composite with higher reinforced phase strength; (2) The interface thickness of the metal matrix composite test sample is in TDTR test range, namely in the thermal penetration range of the light spot; (3) The interface size of the test sample of the metal matrix composite material meets the requirement of TDTR on the size of the test detection light spot; (4) The surface roughness of the test sample of the metal matrix composite material meets the requirement of TDTR test, namely, is smooth enough.
The foregoing embodiments of the present application are not limited to the above embodiments, but are intended to be included within the scope of the present application as defined by the appended claims and their equivalents.
Claims (11)
1. A method of forming an interfacial thermal conductivity test sample, comprising:
Pretreating a material to be detected to obtain a sheet sample, wherein a surface of one side of the sheet sample perpendicular to the thickness direction is used as a target surface, and reinforcing phase particles are arranged in the sheet sample;
selecting the exposed reinforcing phase particles in the target surface as target particles, wherein the exposed surface of the target particles is used as a reference surface;
Placing the sheet sample in a sample inserting groove, and adjusting the included angle between the target surface and the groove bottom to be a preset inclination angle;
injecting a mounting colloid into the mounting groove and solidifying to obtain a mounting sample wrapped with the sheet sample;
Polishing the embedded sample along one side surface of the embedded sample in the direction of the target particles until the distance between a polishing surface and the edge of the reference surface of the target particles is smaller than or equal to a preset distance, so as to obtain a test sample, wherein the polishing surface is used as a tested surface of the test sample;
The polishing the inlaid sample along a side surface of the inlaid sample toward the target particle direction includes: taking the surface of the target particle, which is positioned in the sheet-shaped sample and is adjacent to the reference surface, as a test surface of the target particle, and carrying out polishing along the surface of the embedded sample, which is opposite to the test surface, towards the test surface; an included angle alpha is formed between the reference surface and the test surface, the preset inclination angle is beta, a target included angle between the test surface and the polishing surface of the surface to be tested is theta, and the preset inclination angle is determined according to the following relation: beta=180 ° -alpha-theta.
2. The forming method according to claim 1, characterized by further comprising: and forming a reflecting layer on the polished surface.
3. The method of forming according to claim 1, wherein the test sample is used for TDTR test; the maximum value theta max of the target included angle meets the following conditions: θ is less than or equal to θ max,θmax =arctan (r/H), where r is the spot radius of the laser used in TDTR test, and H is the peak-to-trough amplitude of the topography relief of the measured surface.
4. The method according to claim 3, wherein the roughness of the surface to be measured is 60nm or less, the amplitude H ranges from 200 to 250nm, the spot radius r ranges from 5 to 40 μm, and the target angle θ ranges from 0 ° to 5 °.
5. The method of claim 1, wherein the predetermined distance is in the range of 0-200 nm.
6. The method according to claim 1, wherein the polishing is performed by using two or more polishing wheels from coarse to fine, and sequentially polishing the embedded sample; the mesh number of the selected grinding wheels is 300-200 meshes, and the grinding and polishing rotating speed is 100-250 rpm.
7. The method of forming according to claim 1, wherein the step of injecting and curing the plate-like colloid into the plate-like grooves is performed under normal pressure.
8. An interfacial thermal conductivity test sample formed by the interfacial thermal conductivity test sample formation method of any one of claims 1 to 7, comprising:
The surface of one side of the solidified colloid is covered with a reflecting layer, and the surface of the reflecting layer is used as a surface to be measured;
a sheet sample within the cured gel, the sheet sample having target particles therein;
the target particles have a reference surface and a test surface, the reference surface being exposed to one side surface of the sheet-like sample; the test surface is adjacent to the reference surface, the test surface faces the surface to be tested, and an included angle between the test surface and the surface to be tested is a target included angle, and the target included angle is more than or equal to 0.
9. The interfacial thermal conductivity test sample as defined in claim 8, wherein said test sample is for TDTR testing; the maximum value theta max of the target included angle meets the following conditions: θ is less than or equal to θ max,θmax =arctan (r/H), where r is the spot radius of the laser used in TDTR test, and H is the peak-to-trough amplitude of the topography fluctuation of the measured surface.
10. An interfacial thermal conductivity test sample according to claim 9, wherein said measured surface has a roughness of 60nm or less, said amplitude H ranges from 200 to 250nm, said spot radius r ranges from 5 to 40 μm, and said target included angle θ ranges from 0 ° to 5 °.
11. An interfacial thermal conductivity test sample formed by the method of any one of claims 1 to 7.
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