CN114106711A - Nano-adhesive bonding method for bonding micro device - Google Patents

Nano-adhesive bonding method for bonding micro device Download PDF

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CN114106711A
CN114106711A CN202111407591.0A CN202111407591A CN114106711A CN 114106711 A CN114106711 A CN 114106711A CN 202111407591 A CN202111407591 A CN 202111407591A CN 114106711 A CN114106711 A CN 114106711A
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bonding
samples
sample
pgma
film
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CN114106711B (en
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陈果
易泰民
何小珊
刘艳松
李朝阳
黄景林
王涛
艾星
李俊
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Laser Fusion Research Center China Academy of Engineering Physics
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Laser Fusion Research Center China Academy of Engineering Physics
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C09J5/04Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving separate application of adhesive ingredients to the different surfaces to be joined
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C09J5/06Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving heating of the applied adhesive
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2433/00Presence of (meth)acrylic polymer

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  • Organic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a nano gluing method for bonding a micro device, which comprises the following steps: 1) preparing a glue layer film: depositing a pGMA film on the surface of a sample substrate to be bonded by using an induced water chemical vapor deposition (iCVD) method; 2) activating the glue film: bonding and assembling two to-be-bonded samples coated with pGMA films on a clamping tool, applying appropriate pressure to the samples, soaking the samples in an activating solution EDA (electronic design automation) for 10-20 hours, and ultrasonically cleaning the samples after the activating solution fully activates the pGMA films; 3) curing the activated glue layer film: and (3) assembling the activated and cleaned bonding sample, applying appropriate pressure, air-drying, standing for 70-75 hours, and finishing a curing and crosslinking reaction by the pGMA film to realize bonding of the sample. The gluing method can effectively control the thickness of the gluing glue layer, can realize the gluing of samples with the glue layer thickness of below 500nm at the thinnest, and has very strong binding force among the samples, so that the glued samples are difficult to separate and fall off.

Description

Nano-adhesive bonding method for bonding micro device
Technical Field
The invention relates to the technical field of laser fusion, in particular to a nano gluing method for bonding a micro device.
Background
In laser induced compression science and inertial fusion research, a microstructure target adhered to multiple layers of different materials is impacted by laser. To model and interpret the experiments at high strain rates and laser shock generated pressures, these bond gaps between target layers should be in the submicron range and their bonds should have sufficient strength (bond rupture energy/area ≈ 1 Nm)-1). However, there is a fundamental difficulty in achieving sub-micron liquid glue layers on these tiny components. Despite bonding pressures of 10-100MPa, the bonding gap of liquid glue is typically at least 3 microns and even more than 10 microns, and the glue line thickness is typically greater due to the non-newtonian nature of the squeeze flow during bonding. Laser compression experiments have shown measurable non-ideal effects such as the presence of shock reflections from these non-negligible glue layers, complicating experimental interpretation.
Monomeric Glycidyl Methacrylate (GMA) has epoxy functionality and its iCVD films are often used to bond microfluidic channels or wafers together, and thus, such films are viable for other bonding applications. However, in the conventional method for activating and curing the adhesive layer film, after the adhesive layer film is bonded, the thickness of the adhesive layer between samples is uncontrollable, usually about 10 micrometers, and the thinnest adhesive layer can only be several micrometers. Furthermore, the bonding force between the samples is not strong, and the bonded samples are often separated when the samples are subjected to another process after bonding.
In view of this, the present application is specifically made.
Disclosure of Invention
The invention aims to solve the technical problems that the thickness of an adhesive layer is uncontrollable and the bonding force between samples is not strong in the existing pGMA film activating and curing method, and aims to provide a novel nano-adhesive bonding method for bonding a micro device.
The invention is realized by the following technical scheme:
a nanometer gluing method for adhering tiny devices comprises the following steps: 1) preparing a glue layer film: depositing a glycidyl methacrylate polymer (pGMA) film on the surface of a sample substrate to be bonded by using an Induced Chemical Vapor Deposition (iCVD) method; 2) activating the glue film: bonding and assembling two to-be-bonded samples coated with pGMA films on a clamping tool, applying appropriate pressure to the samples, soaking the samples in an activating solution EDA (electronic design automation) for 10-20 hours, and ultrasonically cleaning the samples after the activating solution fully activates the pGMA films; 3) curing the activated glue layer film: and (3) assembling the activated and cleaned bonding sample, applying appropriate pressure, air-drying, standing for 70-75 hours, and finishing a curing and crosslinking reaction by the pGMA film to realize bonding of the sample.
Currently, the activation of the pGMA film is performed by a gas phase activation method, i.e., a to-be-bonded sample coated with the pGMA film is exposed to the vapor of activated Ethylenediamine (EDA) for about 60 seconds to complete activation, and then a proper pressure is applied at a constant temperature of about 70 ℃, and a pressure of about 10N is usually applied to a sample having a length and a width of 5mm × 5mm, and the sample is left to stand for about 60 minutes to complete the curing and crosslinking reaction of the pGMA film, thereby achieving the bonding of the sample.
The method adopts a liquid phase activation method, namely, a to-be-bonded sample plated with the pGMA film is placed in EDA liquid to be soaked for 10-20 hours, then is cleaned, meanwhile, the bonded sample is always kept under 10N pressure in the cleaning process, then the pressure of about 10N is kept, a fan is used for air drying, and standing is carried out for 72 hours, so that bonding of the sample is realized.
The method can effectively control the thickness of the adhesive layer, can realize the adhesion of samples with the adhesive layer thickness of less than 500nm at the thinnest, and has very strong bonding force among the samples, so that the adhered samples are difficult to separate and fall off.
The specific method of the step 1) comprises the following steps: glycidyl Methacrylate (GMA) is used as a monomer, di-tert-butyl peroxide (DTBP) is used as an initiator, the initiator is fully cracked under the heating condition of a hot wire to induce the polymerization of the GMA monomer, and the pGMA film is deposited on the surface of a cooled sample substrate to be bonded to form the pGMA film.
The ultrasonic cleaning conditions in the step 2) are as follows: 100kHz, 300W, and the washing time is 20 seconds, and the washing is carried out three times in total.
The heating temperature of the hot wire is 190-210 ℃.
The surface temperature of the substrate of the sample to be bonded is 38-42 ℃.
The clamping tool comprises a clamping bottom plate, a supporting rod is vertically arranged on the clamping bottom plate, a clamping pressing block is sleeved on the supporting rod and can move back and forth along the supporting rod towards the clamping bottom plate, the supporting rod is a threaded rod, and the clamping pressing block and the clamping bottom plate are fastened through a nut and the threaded rod.
The invention uses the clamping tool to clamp the sample, applies pressure, can integrally take out the sample after activation, and cleans the sample, can conveniently remove pollutants introduced in the coating and activation processes, and meanwhile, the clamping tool applies pressure by depending on the gravity of an object, namely the self gravity of the clamping pressing block, can ensure the uniformity of the pressure, thereby improving the uniformity of the thickness of the adhesive layer.
And 3) air-drying by adopting a fan.
The flow ratio of GMA to DTBP is GMA: 33%, DTBP: 66 percent.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the embodiment of the invention provides a nano gluing method for gluing a micro device, which can effectively control the thickness of a gluing glue layer, can realize the gluing of samples with the glue layer thickness of below 500nm at the thinnest, and has very strong binding force among samples, so that the glued samples are difficult to separate and fall off;
2. according to the nano gluing method for bonding the micro devices, the clamping tool is used for clamping the sample, pressure is applied, the sample can be taken out integrally after activation, the sample can be cleaned conveniently, pollutants introduced in the coating and activation processes can be removed, meanwhile, the clamping tool applies pressure by means of the gravity of an object, namely the gravity of the clamping pressing block, the uniformity of the pressure can be guaranteed, and therefore the uniformity of the thickness of the glue layer is improved.
Drawings
In order to more clearly illustrate the technical solutions of the exemplary embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and that for those skilled in the art, other related drawings can be obtained from these drawings without inventive effort.
Fig. 1 is a cross-sectional SEM image of a glue layer according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. However, it will be apparent to one of ordinary skill in the art that: it is not necessary to employ these specific details to practice the present invention. In other instances, well-known structures, circuits, materials, or methods have not been described in detail so as not to obscure the present invention.
Throughout the specification, reference to "one embodiment," "an embodiment," "one example," or "an example" means: the particular features, structures, or characteristics described in connection with the embodiment or example are included in at least one embodiment of the invention. Thus, the appearances of the phrases "one embodiment," "an embodiment," "one example" or "an example" in various places throughout this specification are not necessarily all referring to the same embodiment or example. Furthermore, the particular features, structures, or characteristics may be combined in any suitable combination and/or sub-combination in one or more embodiments or examples. Further, those of ordinary skill in the art will appreciate that the illustrations provided herein are for illustrative purposes and are not necessarily drawn to scale. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In the description of the present invention, the terms "front", "rear", "left", "right", "upper", "lower", "vertical", "horizontal", "upper", "lower", "inner", "outer", etc. indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and therefore, should not be construed as limiting the scope of the present invention.
Example 1
As shown in fig. 1, a nano-adhesive bonding method for bonding a micro device according to an embodiment of the present invention includes the following steps: 1) preparing a glue layer film: taking Glycidyl Methacrylate (GMA) as a monomer, taking di-tert-butyl peroxide (DTBP) as an initiator, fully cracking the initiator to induce the polymerization of the GMA monomer under the condition of heating by a hot wire (200 ℃), and depositing on the surface of a cooled to-be-bonded sample substrate (40 ℃) to form a glycidyl methacrylate polymer (pGMA) film; 2) activating the glue film: after assembling the to-be-bonded sample plated with the pGMA film, applying appropriate pressure, usually applying 10N pressure on a sample with the length and width of 5mm multiplied by 5mm, soaking the sample in an activating solution EDA (electronic design automation) liquid for 20 hours, and after the activating solution fully activates the pGMA film, ultrasonically cleaning residual activating solution around the sample; the cleaning conditions are as follows: 100kHz, 300W, the cleaning time is 20 seconds, and the cleaning is carried out three times in total (in the process, the sample to be bonded is always under the pressure of 10N); 3) curing the activated glue layer film: and (3) assembling the activated and cleaned bonding sample, applying proper pressure, air-drying, standing for 72 hours, and finishing a curing and crosslinking reaction of the pGMA film to realize bonding of the sample.
Currently, the activation of the pGMA film is performed by a gas phase activation method, i.e., a to-be-bonded sample coated with the pGMA film is exposed to the vapor of activated Ethylenediamine (EDA) for about 60 seconds to complete activation, and then a proper pressure is applied at a constant temperature of about 70 ℃, and a pressure of about 10N is usually applied to a sample having a length and a width of 5mm × 5mm, and the sample is left to stand for about 60 minutes to complete the curing and crosslinking reaction of the pGMA film, thereby achieving the bonding of the sample.
The method adopts a liquid phase activation method, namely, a to-be-bonded sample plated with a pGMA film is placed in EDA liquid to be soaked for 10-20 hours, then is cleaned, meanwhile, the bonded sample is always kept under 10N pressure in the cleaning process, then the pressure of about 10N is kept, and the bonded sample is air-dried by a fan and stands for 72 hours to realize bonding of the sample.
The method can effectively control the thickness of the adhesive layer, can realize the adhesion of samples with the adhesive layer thickness of less than 500nm at the thinnest, and has very strong bonding force among the samples, so that the adhered samples are difficult to separate and fall off.
Preferably, the ratio of GMA to DTBP is GMA: 33%, DTBP: 66 percent.
As shown in fig. 1, which is an SEM image of the cross-section of the glue layer of the bonding sample prepared in this example, it can be seen that the thickness of the glue layer is relatively uniform and is below 500 nm.
Example 2
The embodiment of the invention provides a preparation method of a nano gluing method for bonding a micro device.
The invention uses the clamping tool to clamp the sample, applies pressure, can integrally take out the sample after activation, and cleans the sample, can conveniently remove pollutants introduced in the coating and activation processes, and meanwhile, the clamping tool applies pressure by depending on the gravity of an object, namely the self gravity of the clamping pressing block, can ensure the uniformity of the pressure, thereby improving the uniformity of the thickness of the adhesive layer.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. A nanometer gluing method for adhering tiny devices is characterized by comprising the following steps: 1) preparing a glue layer film: depositing a glycidyl methacrylate polymer (pGMA) film on the surface of a sample substrate to be bonded by using an Induced Chemical Vapor Deposition (iCVD) method; 2) activating the glue film: bonding and assembling two to-be-bonded samples coated with pGMA films on a clamping tool, applying appropriate pressure to the samples, soaking the samples in an activating solution EDA (electronic design automation) for 10-20 hours, and ultrasonically cleaning the samples after the activating solution fully activates the pGMA films; 3) curing the activated glue layer film: and (3) assembling the activated and cleaned bonding sample, applying appropriate pressure, air-drying, standing for 70-75 hours, and finishing a curing and crosslinking reaction by the pGMA film to realize bonding of the sample.
2. The nano-gluing method for micro device bonding according to claim 1, wherein the specific method of step 1) is as follows: glycidyl Methacrylate (GMA) is used as a monomer, di-tert-butyl peroxide (DTBP) is used as an initiator, the initiator is fully cracked under the heating condition of a hot wire to induce the polymerization of the GMA monomer, and the pGMA film is deposited on the surface of a cooled sample substrate to be bonded to form the pGMA film.
3. The nano-gluing method for tiny device bonding according to claim 1, wherein the ultrasonic cleaning conditions in step 2) are as follows: 100kHz, 300W, and the cleaning time is 20 seconds, and three times are totally cleaned, wherein in the cleaning process, the sample to be bonded is always under proper pressure.
4. The nano-gluing method for micro device bonding as claimed in claim 1, wherein when the sample to be bonded is a sample with a length and a width of 5mm x 5mm, a pressure of 8-10N is applied.
5. The method as claimed in claim 2, wherein the heating temperature of the hot wire is 190-210 ℃.
6. The nano-gluing method for tiny device bonding according to claim 2, wherein the temperature of the surface of the sample substrate to be bonded is 38-42 ℃.
7. The nano-gluing method for bonding micro devices as claimed in claim 1, wherein the clamping tool comprises a clamping base plate, a support rod is vertically arranged on the clamping base plate, a clamping pressing block is sleeved on the support rod, and the clamping pressing block can move back and forth along the support rod towards the clamping base plate.
8. The nano-gluing method for bonding micro devices as claimed in claim 1, wherein the supporting rod is a threaded rod, and the clamping pressing block and the clamping bottom plate are fastened with the threaded rod through nuts.
9. The nano-gluing method for micro device bonding as claimed in claim 1, wherein the air drying is performed by a fan in step 3).
10. The nano-gluing method for micro-device bonding as claimed in claim 2, wherein the flow ratio of GMA and DTBP is GMA: 33%, DTBP: 66 percent.
CN202111407591.0A 2021-11-24 2021-11-24 Nanometer glue connection method for bonding micro devices Active CN114106711B (en)

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CN114106711B CN114106711B (en) 2023-06-27

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102630188A (en) * 2009-09-17 2012-08-08 埃西勒国际通用光学公司 Method and device for chemical vapor deposition of polymer film onto a substrate
CN102666766A (en) * 2009-10-16 2012-09-12 汉高公司 Primer compositions to toughen adhesive bonds
US20140134439A1 (en) * 2012-11-13 2014-05-15 The Research Foundation For The State University Of New York Solvent-less adhesive bonding
KR20180085218A (en) * 2017-01-18 2018-07-26 한국과학기술원 Adhensive thin film and method for adhensive of substrate using the same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102630188A (en) * 2009-09-17 2012-08-08 埃西勒国际通用光学公司 Method and device for chemical vapor deposition of polymer film onto a substrate
CN102666766A (en) * 2009-10-16 2012-09-12 汉高公司 Primer compositions to toughen adhesive bonds
US20140134439A1 (en) * 2012-11-13 2014-05-15 The Research Foundation For The State University Of New York Solvent-less adhesive bonding
KR20180085218A (en) * 2017-01-18 2018-07-26 한국과학기술원 Adhensive thin film and method for adhensive of substrate using the same

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