CN116698907A - Nondestructive pumping-detection heat reflection test method based on film transfer - Google Patents
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- 238000000034 method Methods 0.000 claims abstract description 28
- 238000012360 testing method Methods 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 23
- 150000002739 metals Chemical class 0.000 claims abstract description 15
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 49
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 49
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 49
- 239000010931 gold Substances 0.000 claims description 31
- 239000000758 substrate Substances 0.000 claims description 21
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 239000011521 glass Substances 0.000 claims description 14
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- 230000001066 destructive effect Effects 0.000 claims description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 229910052737 gold Inorganic materials 0.000 claims description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical group [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052594 sapphire Inorganic materials 0.000 claims description 2
- 239000010980 sapphire Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims 18
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims 18
- 238000000576 coating method Methods 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 4
- 239000007769 metal material Substances 0.000 abstract description 2
- 239000013212 metal-organic material Substances 0.000 abstract description 2
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- 238000001755 magnetron sputter deposition Methods 0.000 description 2
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- 238000009659 non-destructive testing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
The invention discloses a nondestructive pumping-detection heat reflection test method based on film transfer. The method can realize that no metal material or organic material remains on the surface after the test. In the coating method, the quality, thickness and interface of each batch of metal films are different. The transfer can ensure the consistency of the quality, thickness and interface condition of the metal film. The method is universal, quick, low in cost and high in repeatability and reliability, and can realize recycling of metals on materials.
Description
Technical Field
The invention relates to the fields of transfer technology and thermal reflection test, in particular to a nondestructive pumping-detection thermal reflection test method based on film transfer.
Background
Pump-probe thermal reflection techniques include Time Domain Thermal Reflection (TDTR), frequency Domain Thermal Reflection (FDTR), transient Thermal Reflection (TTR), steady State Thermal Reflection (SSTR), and the like, which are commonly used for the thermal characterization of electronic device materials (metals, ceramics, semiconductors, etc.). The pumping light source heats the surface of the sample, and the surface is subjected to temperature change; detecting the change of the reflectivity of the laser detection surface, and indirectly detecting the change of the surface temperature by a detection laser according to the principle of thermal reflection (the change of the reflectivity is in direct proportion to the temperature); the thermal property information of the material is hidden behind the temperature change, and the thermal properties (heat conductivity and interface thermal resistance) of the multilayer material are fitted by combining a thermal conduction model. In order to satisfy the linear relation between the reflectivity change and the temperature change, metal is usually plated on the surface of the material, because most metals such as Au and Al satisfy good linearity; the surface metal ensures that the light of the heating laser is sufficiently absorbed and converted into heat. Common coating methods include thermal evaporation, electron beam evaporation, magnetron sputtering and the like, which can form good bonding force between the material and the metal film, but the metal can be diffused into the material to form a mixed layer in the testing process to damage the material, so that the method cannot be applied to a rapid production line.
Disclosure of Invention
The traditional heat reflection technology has destructiveness to materials under the condition of using a metal film, and aims at the fact that the metal film of a transition substrate in the prior art adopts Polydimethylsiloxane (PDMS) to assist in transferring to transfer to a sample to be tested, the main purpose of the invention is to provide a nondestructive testing technology based on film transferring, and to realize recycling of the metal film, and the nondestructive pumping-detection heat reflection testing method is more universal, rapid and low in cost, and realizes recycling of metal on the surface of the material.
In order to achieve the above object, the present invention provides a nondestructive pumping-detection heat reflection test method based on film transfer, which is characterized in that: the method comprises the following steps:
s1: plating a layer of metal film on the transition substrate, wherein the thickness of the film needs to be calibrated;
s2: covering PDMS above the metal film, and controlling the temperature within the range of normal temperature to 200 ℃; the PDMS is prepared by mixing and curing a main agent, namely glue A, and a hardening agent, namely glue B;
s3: after contacting the slide with PDMS, squeezing the slide;
s4: peeling the metal film by PDMS;
s5: placing a sample to be tested; fully contacting the metal film with a sample to be detected, and extruding the glass slide at the temperature of normal temperature to 200 ℃;
s6: the metal film is separated from the PDMS and transferred to the sample;
s7: measuring the thickness, roughness and folds of the metal film, and determining the area for testing after transfer;
s8: carrying out pumping-detection heat reflection test on a sample to be tested by using the transferred metal film;
s9: repeating the steps S2-S4 on the metal film after the test is finished, and transferring the metal on the sample to be tested; thereafter, cleaning the sample surface;
s10: the surface of the sample was analyzed to verify whether there was residue.
The method comprises the following specific steps:
step S1: a layer of metal film is plated on a transition substrate, the substrate can be various flat substrates such as silicon (Si), sapphire, silicon dioxide/silicon (SiO 2/Si) and the like, and the metal film can be single-layer metal such as gold (Au), aluminum (Al), copper (Cu), platinum (Pt) and the like, and the thickness of the film needs to be calibrated. Common coating methods include thermal evaporation, electron beam evaporation, magnetron sputtering, and the like.
Step S2: covering PDMS on the metal film, controlling the temperature to be in the range of normal temperature to 200 ℃, preferably 150 ℃; the PDMS is prepared by mixing a main agent (adhesive A) and a hardening agent (adhesive B) and curing; preferably, PDMS is covered on the metal film, and the temperature is 150 ℃; the mass ratio of the adhesive A to the adhesive B is 10:1.
Step S3: using a micro-motion platform to adhere the slide below the platform, slowly descending until the slide is in complete contact with the PDMS, and extruding the slide for 0-20 minutes; preferably, the slide is pressed for a period of 5-10 minutes.
Step S4: the platform was quickly raised and the PDMS and glass plate were lifted together while the PDMS peeled off the metal film.
The second scheme of step S4: siO is selected in step S1 2 with/Si as substrate, PDMS/gold film/SiO obtained by steps S2-S3 2 The whole structure of Si is put into a strong acid or alkali solution, wherein the strong acid or alkali is not more than 1% hydrofluoric acid (HF) or sodium hydroxide solution (NaOH). The strong acid or alkali solution etches the sacrificial layer SiO 2 PDMS adheres to the metal, separating from Si. The key point of selecting strong acid or strong alkali in the invention is that: strong acid or strong base and SiO 2 Chemical reaction occurs but does not react with PDMS or metals; can etch SiO 2 So that PDMS/metal is combined withAnd separating the Si substrate.
For metals Au and Pt with poor adhesion, the preparation of the PDMS/metal film is realized by utilizing the steps S1 to S4;
for metals with good adhesion, such as Al and Ni, a layer of metals with poor adhesion (Au and Pt) of about 1nm (1 nm-5 nm) can be plated between the metals and the transition substrate, and then the preparation of the PDMS/multilayer metal film is realized by utilizing the steps S1-S4. In addition, any metal species can be realized with the second scheme of steps S1-S4.
Step S5: placing a sample to be tested, wherein the sample to be tested comprises a single-layer material or any material such as a multi-layer film material. Slowly lowering the platform to make the PDMS/metal film close to the sample until the metal film is fully contacted with the sample to be detected, and extruding the slide at normal temperature to 200 ℃ for 0-20 minutes; preferably, the slide is extruded at normal temperature to 200℃for 5-10 minutes.
Step S6: the platform was slowly raised and the PDMS and glass were raised together while the metal film was transferred off the PDMS onto the sample.
Step S7: the thickness, roughness and wrinkles of the metal film were measured using an Atomic Force Microscope (AFM) to determine the areas that could be used for testing after transfer.
Step S8: and carrying out a pump-detection heat reflection test on the sample to be tested by using the transferred metal film.
Step S9: and after the test is finished, repeating the steps S2-S4 on the metal film, and transferring the metal on the sample to be tested. Thereafter, the sample surface was cleaned with acetone. Preferably, the cleaning step is: ultrasonic cleaning and then drying; after the washing with acetone was completed, the washing was repeated with isopropyl alcohol using the same procedure.
Step S10: and analyzing the surface of the sample by using high-power microscope, raman spectrum, fluorescence spectrum, AFM and other tests to verify whether residues exist. The Raman spectrum and the fluorescence spectrum can see signals of different materials through peaks, and the high-power microscope and the AFM can directly observe the surface structure.
Compared with the prior art, the invention has the following advantages:
the method has the outstanding advantages of repeatability, namely the same result can be obtained by transferring for multiple times; the reliability, i.e. the sample obtained by the method can successfully finish the subsequent heat reflection test. The method comprises the following steps:
1. compared with the traditional film plating method, the method can realize that no metal material or organic material remains on the surface after the test.
2. In the coating method, the quality, thickness and interface of each batch of metal films are different. The transfer can ensure the consistency of the quality, thickness and interface condition of the metal film.
3. The method is universal, quick, low in cost and high in repeatability and reliability, and can realize recycling of metals on materials.
Drawings
FIG. 1 is a schematic diagram showing the process of steps S1 to S2 in embodiment 1 of the present invention;
FIG. 2 is a schematic diagram showing the process of steps S3 to S4 in embodiment 1 of the present invention;
FIG. 3 is a schematic diagram showing the process of steps S5 to S6 in embodiment 1 of the present invention;
FIG. 4 is a schematic diagram of a material structure of the present invention in which a layer of Au (about 1nm, or 1nm-5 nm) is plated between a metal and a transition substrate according to example 2;
fig. 5 is a schematic diagram illustrating the process of steps S2 to S3 in embodiment 3 of the present invention.
Detailed Description
In order to better understand the above technical solutions, the following detailed description will refer to the accompanying drawings and specific embodiments.
Example 1
A non-destructive pumping-detection heat reflection test method, see fig. 1 and 2, comprising the steps of:
step S1: a Au thin film 20 is plated on the transition substrate 10. Specifically, the thickness of the Au thin film was 80nm.
Step S2: polydimethylsiloxane (PDMS) 30 was covered over Au thin film 20 and placed on heating table 40. Specifically, PDMS30 is prepared by mixing a main agent (adhesive A) and a hardening agent (adhesive B) in a ratio of 10:1 and curing. The area should be smaller than that of the Au thin film 20, and the temperature of the heating stage is controlled at 150 ℃.
Step S3: the glass sheet 50 is adhered under the micro stage 60 and slowly lowered until it is completely contacted with the PDMS30, and the glass sheet is pressed for a certain time. Specifically, the temperature was controlled at 150℃and the extrusion time was 5 minutes.
Step S4: the micro-stage 60 is rapidly raised and the pdms30 is raised together with the glass sheet 50 while the PDMS30 peels off the Au thin film 20.
Step S5: placing the sample 70 to be tested, slowly lowering the micro-motion platform 60 to enable the PDMS30/Au film 20 to be close to the sample 70 to be tested until the Au film 20 is fully contacted with the sample 70 to be tested, and extruding the glass sheet 50. Specifically, the sample to be measured 70 includes any material such as a single layer material, or a multi-layer film material. This step was carried out at 150℃and the extrusion time was 5 minutes.
Step S6: slowly raise micro-motion stage 60, PDMS30 and glass sheet 50 are raised together, and Au thin film 20 is transferred to sample 70 to be measured off PDMS 30.
Step S7: the thickness, roughness, and wrinkles of the Au thin film 20 were measured using an Atomic Force Microscope (AFM) to determine the area that could be used for testing after transfer.
Step S8: the sample 70 to be tested is subjected to a pump-probe thermal reflection test using the transferred Au thin film 20.
Step S9: after the test is completed, steps S2 to S4 are repeated for the Au thin film 20 to transfer Au on the sample 70 to be tested. Thereafter, the sample surface was cleaned with acetone. The cleaning steps are as follows: ultrasonic cleaning and then drying. After the washing with acetone was completed, the washing was repeated with isopropyl alcohol using the same procedure.
Step S10: and analyzing the surface of the sample by using high-power microscope, raman spectrum, fluorescence spectrum, AFM and other tests to verify whether residues exist. The Raman spectrum and the fluorescence spectrum can see signals of different materials through peaks, and the high-power microscope and the AFM can directly observe the surface structure.
Example 2
Example 2 provides another method of non-destructive pumping-detection thermal reflection test, and example 2 is different from example 1 in that the metal film used in example 2 has an Al structure, and the bonding force between Al and the transition substrate is strong, so that the transfer is assisted by an Au layer with weak bonding force. Referring to fig. 2, 3 and 4, the method comprises the steps of:
step S1: an Al/Au thin film 20 is plated on the transition substrate 10. Specifically, the Al film 21 in the Al/Au film 20 has a thickness of 80nm and the Au film 22 has a thickness of 1nm.
Step S2: a Polydimethylsiloxane (PDMS) 30 was covered on the Al thin film 21 and placed on a heating stage 40. Specifically, PDMS30 is prepared by mixing a main agent (adhesive A) and a hardening agent (adhesive B) in a ratio of 10:1 and curing. The area should be smaller than that of the Al/Au thin film 20, and the temperature of the heating stage is controlled at 150 ℃.
Step S3: the glass sheet 50 is adhered under the micro stage 60 and slowly lowered until it is completely contacted with the PDMS30, and the glass sheet is pressed for a certain time. Specifically, the temperature was controlled at 150℃and the extrusion time was 5 minutes.
Step S4: the micro-stage 60 is rapidly raised and the PDMS30 is raised together with the glass sheet 50 while the PDMS30 peels off the Al/Au thin film 20.
The subsequent steps are substantially the same as those of steps S5 to S10 in example 1, except that the peeled and transferred film is an Al/Au film, and the Al film is smoothly transferred by means of a relatively low bonding force of the Au film.
Example 3
Example 3 provides yet another method of non-destructive pumping-probe thermal reflection testing, example 3 differs from the first two embodiments in that example 3 uses a dry-wet mixing method to transfer the metal film, and etches the sacrificial layer using an acid-base solution, thereby stripping the PDMS, metal film, and transition substrate. Referring to fig. 5, the method comprises the steps of:
step S1: in SiO 2 An Al film 20 is plated on the Si substrate 10. Specifically, the thickness of the Al film was 80nm.
Step S2: polydimethylsiloxane (PDMS) 30 was overlaid on Al thin film 20 and placed in HF solution 40 at 1% concentration. Specifically, PDMS30 is prepared by mixing a main agent (adhesive A) and a hardening agent (adhesive B) in a ratio of 10:1 and curing. The area should be smaller than that of the Al thin film 20.
Step S3: after soaking for a period of time, siO 2 The etched PDMS30 is peeled off from the Si substrate 10 by adhering the combined structure of the Al thin film 20. The combined structure floats in solution 40.
Step S4: taking out the combined structure and cleaning and drying the combined structure.
The following steps are substantially the same as steps S5 to S10 in example 1, except that the peeled and transferred film is an Al film. The binding force between the transferred Al film and the sample to be measured is far smaller than that between Al film obtained by directly coating and the transition sample, so that the transferring step can directly utilize PDMS to transfer without using an acid-base solution.
In summary, the embodiments of the present invention are not limited to the above 1-3, and the same and reliable results have been obtained through a plurality of experiments, thereby confirming that the method of the present invention is highly repeatable and reliable.
Claims (9)
1. A nondestructive pumping-detection heat reflection testing method based on film transfer is characterized in that: the method comprises the following steps:
s1: plating a layer of metal film on the transition substrate, wherein the thickness of the film needs to be calibrated;
s2: covering PDMS above the metal film, and controlling the temperature within the range of normal temperature to 200 ℃; the PDMS is prepared by mixing and curing a main agent, namely glue A, and a hardening agent, namely glue B;
s3: after contacting the slide with PDMS, squeezing the slide;
s4: peeling the metal film by PDMS;
s5: placing a sample to be tested; fully contacting the metal film with a sample to be detected, and extruding the glass slide at the temperature of normal temperature to 200 ℃;
s6: the metal film is separated from the PDMS and transferred to the sample;
s7: measuring the thickness, roughness and folds of the metal film, and determining the area for testing after transfer;
s8: carrying out pumping-detection heat reflection test on a sample to be tested by using the transferred metal film;
s9: repeating the steps S2-S4 on the metal film after the test is finished, and transferring the metal on the sample to be tested; thereafter, cleaning the sample surface;
s10: the surface of the sample was analyzed to verify whether there was residue.
2. The film transfer-based non-destructive pumping-detection thermal reflection test method of claim 1, wherein: the method comprises the following specific steps:
the step S1: plating a metal film on a transition substrate, wherein the substrate is silicon, sapphire or silicon dioxide/silicon, the metal film is gold, aluminum, copper or platinum single-layer metal, and the thickness of the film needs to be calibrated;
the step S2: covering PDMS above the metal film, and controlling the temperature within the range of normal temperature to 200 ℃; the PDMS is prepared by mixing and curing a main agent, namely glue A, and a hardening agent, namely glue B;
the step S3: using a micro-motion platform to adhere the slide below the platform, slowly descending until the slide is in complete contact with the PDMS, and extruding the slide for 0-20 minutes;
the step S4: the platform is quickly lifted, the PDMS and the glass sheet are lifted together, and the metal film is peeled off by the PDMS;
the step S5: placing a sample to be tested, wherein the sample to be tested comprises a single-layer material or a multi-layer film material; slowly lowering the platform to make the PDMS/metal film close to the sample until the metal film is fully contacted with the sample to be detected, and extruding the slide at normal temperature to 200 ℃ for 0-20 minutes;
the step S6: slowly lifting the platform, and lifting the PDMS and the glass together, wherein the metal film is separated from the PDMS and is transferred to the sample;
the step S7: measuring the thickness, roughness and folds of the metal film by utilizing an Atomic Force Microscope (AFM), and determining the area for testing after transfer;
the step S8: carrying out pumping-detection heat reflection test on a sample to be tested by using the transferred metal film;
the step S9: repeating the steps S2-S4 on the metal film after the test is finished, and transferring the metal on the sample to be tested; thereafter, the sample surface was cleaned with acetone;
the step S10: analyzing the surface of the sample by using a high-power microscope, a Raman spectrum, a fluorescence spectrum or an AFM test to verify whether residues exist; wherein the Raman spectrum and the fluorescence spectrum can see signals of different materials through wave peaks, and the high power microscope and the AFM directly observe the surface structure.
3. The film transfer-based non-destructive pumping-detection thermal reflection test method of claim 2, wherein: in the step S2: covering PDMS above the metal film at 150deg.C; the mass ratio of the adhesive A to the adhesive B is 10:1.
4. A non-destructive pumping-detection thermal reflection test method based on film transfer according to claim 3, wherein: in the step S3: the slide was extruded for 5-10 minutes.
5. The film transfer-based non-destructive pumping-detection thermal reflection test method of claim 4, wherein: in the step S4: siO is selected in step S1 2 with/Si as substrate, PDMS/gold film/SiO obtained by steps S2-S3 2 Placing the whole structure of Si into strong acid or strong alkali solution, wherein the strong acid or strong alkali is hydrofluoric acid or sodium hydroxide solution with concentration of not more than 1%; the strong acid or alkali solution etches the sacrificial layer SiO 2 PDMS adheres to the metal, separating from the Si substrate.
6. The film transfer-based non-destructive pumping-detection thermal reflection test method of claim 5, wherein: in the step S5: the slide was extruded at room temperature to 200℃for 5-10 minutes.
7. The film transfer-based non-destructive pumping-detection thermal reflection test method of claim 6, wherein: in the step S9: the cleaning steps are as follows: ultrasonic cleaning and then drying; after the washing with acetone was completed, the washing was repeated with isopropyl alcohol using the same procedure.
8. The film transfer-based non-destructive pumping-detection thermal reflection test method according to any one of claims 1 to 7, wherein: for metals Au and Pt with poor adhesion, the preparation of the PDMS/metal film is realized by utilizing the steps S1-S4.
9. The film transfer-based non-destructive pumping-detection thermal reflection test method according to any one of claims 1 to 7, wherein:
for metals Al and Ni with good adhesion, plating a layer of metals Au and Pt with poor adhesion of 1nm-5nm between the metals and the transition substrate, and then utilizing the steps S1-S4 to prepare the PDMS/multilayer metal film so as to strip the metals with good adhesion by means of the metals with poor adhesion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310647939.6A CN116698907A (en) | 2023-05-30 | 2023-05-30 | Nondestructive pumping-detection heat reflection test method based on film transfer |
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