Single-component target binding copper adhesive and preparation method thereof

Abstract

This invention provides a single-component copper-bonding adhesive for target bonding and its preparation method, belonging to the field of target bonding technology. The method involves adding an epoxy room-temperature curing agent and hydrogenated castor oil to a modified solution, stirring until completely dissolved to obtain a modified curing agent solution; then adding epoxy resin, conductive filler, and coupling agent to the modified curing agent solution, dispersing and defoaming to obtain the final product. The resulting copper-bonding adhesive is a single-component adhesive, avoiding glue flow and eliminating the need to introduce silver powder or silver-coated copper powder as conductive and thermally conductive fillers, significantly reducing costs.

Description

Technical Field

[0001] This invention belongs to the field of target bonding technology, and particularly relates to a single-component target bonding copper adhesive and its preparation method. Background Technology

[0002] Target bonding is a technique that binds a target material to a backing plate. The integrity and bonding rate of the target-backing plate bond determine the target's performance and cost, therefore the requirements for target bonding are relatively high. Using bonding adhesives to bond targets is a relatively low-cost technique. This method uses special thermally and electrically conductive adhesives to bond the target material to the backing plate.

[0003] Currently, most target bonding adhesives are prone to flow in sealed environments. While these two-component adhesives offer the advantage of long shelf life, the bonding process is cumbersome and requires strict control over the ratio of the two components. Furthermore, most bonding adhesives currently use silver powder or silver-plated copper powder as conductive fillers, resulting in higher costs and hindering cost control of target materials.

[0004] Therefore, it is necessary to improve the existing technology in order to address the shortcomings of the existing technology.

[0005] In view of this, the present invention is hereby proposed. Summary of the Invention

[0006] The purpose of this invention is to provide a single-component target bonding copper adhesive and its preparation method, which realizes the use of a single component as a bonding adhesive and avoids the phenomenon of adhesive flow. It eliminates the need to introduce silver powder or silver-coated copper powder as conductive and thermally conductive fillers, thus greatly reducing costs.

[0007] To achieve the above objectives, this application adopts the following technical solution:

[0008] A method for preparing a single-component target-bonded copper adhesive involves adding an epoxy room-temperature curing agent and hydrogenated castor oil to a modified solution and stirring until completely dissolved to obtain a modified curing agent solution; then adding epoxy resin, conductive filler, and coupling agent to the modified curing agent solution, dispersing and defoaming to obtain the final product.

[0009] Further, according to the parts by weight, the modified solution, epoxy room temperature curing agent, hydrogenated castor oil, epoxy resin, conductive filler and coupling agent are 11-15 parts, 0.3-0.6 parts, 0.8-1.2 parts, 8-12 parts, 72-75 parts and 0.3-0.6 parts respectively.

[0010] By adding the combination of epoxy room temperature curing agent and hydrogenated castor oil, and after modification with a modified solution, the bonding adhesive becomes a solvent-evaporating curing adhesive. It will not cure when the curing agent contains solvent, that is, it will not cure before bonding. After the solvent gradually evaporates, the bonding adhesive will slowly cure, and complete curing will be achieved after 24 hours, thus achieving the purpose of making the bonding adhesive a single component.

[0011] Preferably, when adding epoxy resin, conductive filler and coupling agent, a metal surface passivating agent is also added simultaneously; further, the metal surface passivating agent is 0.3 to 2.2 parts by weight.

[0012] Preferably, the metal surface passivating agent may include ammonium dichromate. Because the addition of a metal surface passivating agent, especially ammonium dichromate, decomposes into Cr2O3 and N2 at 180°C, the nitrogen can form a nitrogen protective layer on the adhesive surface, and the chromium oxide can form a passivation protective film on the copper surface, preventing the copper from directly contacting air and oxidizing. This is sufficient to provide passivation at the target's operating temperature of around 250°C, further forming protection. Consequently, the bonding adhesive does not need to introduce silver powder or silver-coated copper powder as conductive and thermally conductive fillers, significantly reducing costs.

[0013] Preferably, an oxygen-supplying agent is added simultaneously with the epoxy resin, conductive filler, and coupling agent; further, the oxygen-supplying agent is 0.3 to 0.6 parts by weight.

[0014] Preferably, the oxygen-supplying agent includes one or more of copper nitrate, silver nitrate, or silver oxide. Introducing the oxygen-supplying agent causes it to decompose upon heating, generating metal and oxygen. The oxygen provides oxygen for the curing process in a closed environment, preventing adhesive run-off during bonding. Simultaneously, the metal enhances the conductivity of the bonding adhesive, creating a dual-benefit effect.

[0015] Furthermore, the modified solution comprises a mixed solution of butyl glycidyl ether and butanone.

[0016] Preferably, the butyl glycidyl ether and butanone are 3-5 parts and 8-10 parts by weight, respectively.

[0017] Furthermore, the epoxy room temperature curing agent includes one or more of ethylenediamine, diethylenetriamine, or triethylenetetramine.

[0018] Preferably, the epoxy resin includes one of bisphenol A type epoxy resin E-51, bisphenol A type epoxy resin E-44, or bisphenol F type epoxy resin F-170.

[0019] Preferably, the conductive filler comprises spherical copper powder.

[0020] The present invention also provides a single-component target-bonded copper adhesive prepared by the preparation method described above.

[0021] Compared with existing technologies, this application uses a combination of epoxy room temperature curing agent and hydrogenated castor oil as curing agents, and after modification, achieves the bonding adhesive as a single component; at the same time, it introduces oxygen supply agents and passivating agents to avoid glue flow and reduce costs. Attached Figure Description

[0022] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments will be briefly described below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation on the scope of this application.

[0023] Figure 1 This is a SEM image of the single-component target material bonded to copper adhesive in Example 1 of the present invention.

[0024] Figure 2 This is a physical image of the single-component target material bonded with copper adhesive according to Embodiment 1 of the present invention. Detailed Implementation

[0025] The implementation schemes of this application will be described in detail below with reference to specific embodiments. However, those skilled in the art will understand that the following embodiments are only for illustrating this application and should not be regarded as limiting the scope of this application. Unless otherwise specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments used without specified manufacturers are all conventional products that can be purchased commercially.

[0026] Example 1

[0027] A method for preparing a single-component target-bonded copper adhesive:

[0028] (1) Weigh 4 parts of butyl glycidyl ether and 9 parts of butanone according to the weight, mix them evenly, then add 1 part of hydrogenated castor oil CO-40 and 0.5 parts of ethylenediamine, and stir at a stirring speed of 2000 rpm until completely dissolved to obtain the modified curing agent solution.

[0029] (2) According to the weight parts, 10 parts of bisphenol A type epoxy resin E-51, 74 parts of spherical copper powder conductive filler, 0.5 parts of silane coupling agent KH560, 0.5 parts of copper nitrate and 0.5 parts of ammonium dichromate were added to the modified curing agent solution in step (1). After dispersion and defoaming in a centrifuge, a single-component target-bonded copper adhesive was obtained, the microstructure of which is shown in […]. Figure 1 As shown in the image, a physical picture of a single-component target bonded with copper adhesive is shown below. Figure 2 As shown.

[0030] Example 2

[0031] A method for preparing a single-component target-bonded copper adhesive:

[0032] (1) Weigh 4 parts of butyl glycidyl ether and 9 parts of butanone according to the weight, mix them evenly, then add 1 part of hydrogenated castor oil CO-40 and 0.5 parts of diethylenetriamine, and stir at a stirring speed of 2000 rpm until completely dissolved to obtain the modified curing agent solution.

[0033] (2) According to the weight parts, 10 parts of bisphenol A type epoxy resin E-44, 74 parts of spherical copper powder conductive filler, 0.5 parts of silane coupling agent KH560, 0.5 parts of silver nitrate and 0.5 parts of ammonium dichromate are added to the modified curing agent solution in step (1). After dispersion and defoaming in a centrifuge, a single-component target bonding copper adhesive is obtained.

[0034] Example 3

[0035] A method for preparing a single-component target-bonded copper adhesive:

[0036] (1) Weigh 4 parts of butyl glycidyl ether and 9 parts of butanone according to the weight, mix them evenly, then add 1 part of hydrogenated castor oil CO-40 and 0.5 parts of triethylenetetramine, and stir at a stirring speed of 2000 rpm until completely dissolved to obtain the modified curing agent solution.

[0037] (2) According to the weight parts, 10 parts of bisphenol F type epoxy resin F-170, 74 parts of spherical copper powder conductive filler, 0.5 parts of silane coupling agent KH560, 0.5 parts of silver oxide and 0.5 parts of ammonium dichromate are added to the modified curing agent solution in step (1). After dispersion and defoaming in a centrifuge, a single-component target material bonding copper glue is obtained.

[0038] Example 4

[0039] A method for preparing a single-component target-bonded copper adhesive:

[0040] (1) Weigh 4 parts of butyl glycidyl ether and 9 parts of butanone according to the weight, mix them evenly, then add 1 part of hydrogenated castor oil CO-40 and 0.5 parts of triethylenetetramine, and stir at a stirring speed of 2000 rpm until completely dissolved to obtain the modified curing agent solution.

[0041] (2) According to the weight parts, 10 parts of bisphenol F type epoxy resin F-170, 73.5 parts of spherical copper powder conductive filler, 0.5 parts of silane coupling agent KH560, 0.5 parts of copper nitrate and 1 part of ammonium dichromate are added to the modified curing agent solution in step (1). After centrifugation and defoaming, a single-component target material bonding copper adhesive is obtained.

[0042] Example 5

[0043] A method for preparing a single-component target-bonded copper adhesive:

[0044] (1) Weigh 4 parts of butyl glycidyl ether and 9 parts of butanone according to the weight, mix them evenly, then add 1 part of hydrogenated castor oil CO-40 and 0.5 parts of triethylenetetramine, and stir at a stirring speed of 2000 rpm until completely dissolved to obtain the modified curing agent solution.

[0045] (2) According to the weight parts, 10 parts of bisphenol F type epoxy resin F-170, 72.5 parts of spherical copper powder conductive filler, 0.5 parts of silane coupling agent KH560, 0.5 parts of copper nitrate and 2 parts of ammonium dichromate are added to the modified curing agent solution in step (1). After dispersion and defoaming in a centrifuge, a single-component target material bonding copper adhesive is obtained.

[0046] Example 6

[0047] A method for preparing a single-component target-bonded copper adhesive:

[0048] (1) Weigh 4 parts of butyl glycidyl ether and 9 parts of butanone according to the weight, mix them evenly, then add 1 part of hydrogenated castor oil CO-40 and 0.5 parts of triethylenetetramine, and stir at a stirring speed of 2000 rpm until completely dissolved to obtain the modified curing agent solution.

[0049] (2) According to the weight parts, add 10 parts of bisphenol A type epoxy resin E-51, 74 parts of spherical copper powder conductive filler, 0.5 parts of silane coupling agent KH560 and 1 part of ammonium dichromate to the modified curing agent solution in step (1). After centrifugation and defoaming, a single-component target material bonding copper glue is obtained.

[0050] Example 7

[0051] A method for preparing a single-component target-bonded copper adhesive:

[0052] (1) Weigh 4 parts of butyl glycidyl ether and 9 parts of butanone according to the weight, mix them evenly, then add 1 part of hydrogenated castor oil CO-40 and 0.5 parts of triethylenetetramine, and stir at a stirring speed of 2000 rpm until completely dissolved to obtain the modified curing agent solution.

[0053] (2) According to the weight parts, add 10 parts of bisphenol A type epoxy resin E-51, 74 parts of spherical copper powder conductive filler, 0.5 parts of silane coupling agent KH560 and 1 part of copper nitrate to the modified curing agent solution in step (1). After centrifugation and defoaming, a single-component target material bonding copper glue is obtained.

[0054] Example 8

[0055] A method for preparing a single-component target-bonded copper adhesive:

[0056] (1) Weigh 4 parts of butyl glycidyl ether and 9 parts of butanone according to the weight, mix them evenly, then add 1 part of hydrogenated castor oil CO-40 and 0.5 parts of triethylenetetramine, and stir at a stirring speed of 2000 rpm until completely dissolved to obtain the modified curing agent solution.

[0057] (2) According to the weight parts, add 10 parts of bisphenol A type epoxy resin E-51, 75 parts of spherical copper powder conductive filler and 0.5 parts of silane coupling agent KH560 to the modified curing agent solution in step (1). After dispersion and defoaming in a centrifuge, a single-component target material bonding copper glue is obtained.

[0058] Example 9

[0059] A method for preparing a single-component target-bonded copper adhesive:

[0060] (1) Weigh 5 parts of butyl glycidyl ether and 8 parts of butanone according to the weight, mix them evenly, then add 1.2 parts of hydrogenated castor oil CO-40 and 0.3 parts of ethylenediamine, and stir at a stirring speed of 2000 rpm until completely dissolved to obtain the modified curing agent solution.

[0061] (2) According to the weight parts, add 9 parts of bisphenol A type epoxy resin E-51, 75 parts of spherical copper powder conductive filler, 0.5 parts of silane coupling agent KH560, 0.5 parts of copper nitrate and 0.5 parts of ammonium dichromate to the modified curing agent solution in step (1). After centrifugation and defoaming, a single-component target bonding copper adhesive is obtained.

[0062] Example 10

[0063] A method for preparing a single-component target-bonded copper adhesive:

[0064] (1) Weigh 5 parts of butyl glycidyl ether and 8 parts of butanone according to the weight, mix them evenly, then add 0.8 parts of hydrogenated castor oil CO-40 and 0.7 parts of ethylenediamine, and stir at a stirring speed of 2000 rpm until completely dissolved to obtain the modified curing agent solution.

[0065] (2) According to the weight parts, 11 parts of bisphenol A type epoxy resin E-51, 73 parts of spherical copper powder conductive filler, 0.5 parts of silane coupling agent KH560, 0.5 parts of copper nitrate and 0.5 parts of ammonium dichromate are added to the modified curing agent solution in step (1). After dispersion and defoaming in a centrifuge, a single-component target material bonding copper adhesive is obtained.

[0066] Comparative Example 1

[0067] A method for preparing a two-component target-bonded copper adhesive:

[0068] (1) Preparation of component A

[0069] According to the weight parts, take 75.5 parts of spherical copper powder conductive filler, 4 parts of butyl glycidyl ether, 19 parts of diethylene glycol butyl ether acetate, 1 part of curing agent ethylenediamine and 0.5 parts of silane coupling agent KH560, and after centrifugation and defoaming, obtain component A of the two-component target material bonding copper adhesive.

[0070] (2) Preparation of component B

[0071] According to the weight proportions, take 20 parts of bisphenol A type epoxy resin E-51, 75.5 parts of spherical copper powder conductive filler, 4 parts of butyl glycidyl ether and 0.5 parts of silane coupling agent KH560, and after centrifugation and defoaming, obtain the B component of the two-component target material bonding copper adhesive.

[0072] (3) Mix the A component and B component obtained in steps (1) and (2) at a mass ratio of 1:1 to obtain a two-component target bonding copper adhesive.

[0073] Table 1 shows a comparison of the performance tests of the copper pastes obtained in the examples and comparative examples.

[0074] Table 1 Comparison of performance tests of copper adhesives obtained in Examples 1-11 and Comparative Example 1

[0075]

[0076] As can be seen from Table 1, in Example 6, no oxygen supply agent was added, resulting in incomplete curing of the colloid and partial glue flow, which affected both resistivity and shear strength. In Example 7, no metal passivator was added, which made it prone to oxidation at high temperatures, leading to a significant increase in resistivity after 250℃ / 1h. In Example 8, both oxygen supply agent and metal passivator were lacking, and all parameters were significantly affected.

[0077] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.

[0078] Furthermore, those skilled in the art will understand that although some embodiments herein include certain features included in other embodiments but not others, combinations of features from different embodiments are intended to be within the scope of this application and form different embodiments. For example, in the foregoing claims, any of the claimed embodiments can be used in any combination. The information disclosed in this background section is intended only to enhance the understanding of the general background of this application and should not be construed as an admission or in any way implying that such information constitutes prior art known to those skilled in the art.

Claims

1. A method for preparing a single-component target-bonded copper adhesive, characterized in that, Add epoxy room temperature curing agent and hydrogenated castor oil to the modified solution and stir until completely dissolved to obtain a modified curing agent solution; add epoxy resin, conductive filler, coupling agent, metal surface passivator and oxygen supply agent to the modified curing agent solution, disperse and defoam, and the product is obtained. The modified solution comprises a mixed solution of butyl glycidyl ether and butanone; The conductive filler includes spherical copper powder; The metal surface passivating agent includes ammonium dichromate; The oxygen-supplying agent includes one or more of copper nitrate, silver nitrate, or silver oxide.

2. The method for preparing single-component target-bonded copper adhesive according to claim 1, characterized in that, According to the weight parts, the modified solution, epoxy room temperature curing agent, hydrogenated castor oil, epoxy resin, conductive filler and coupling agent are 11-15 parts, 0.3-0.6 parts, 0.8-1.2 parts, 8-12 parts, 72-75 parts and 0.3-0.6 parts respectively.

3. The method for preparing single-component target-bonded copper adhesive according to claim 2, characterized in that, The metal surface passivating agent is used in amounts of 0.3 to 2.2 parts by weight.

4. The method for preparing single-component target-bonded copper adhesive according to claim 3, characterized in that, The oxygen supply agent is 0.3 to 0.6 parts by weight.

5. The method for preparing single-component target-bonded copper adhesive according to claim 2, characterized in that, The butyl glycidyl ether and butanone are 3-5 parts and 8-10 parts by weight, respectively.

6. The method for preparing single-component target-bonded copper adhesive according to claim 1 or 2, characterized in that, The epoxy room temperature curing agent includes one or more of ethylenediamine, diethylenetriamine, or triethylenetetramine.

7. A single-component target-bonded copper adhesive prepared by the preparation method according to any one of claims 1-6.

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