CN112980364A - Temporary bonding glue with high thermal stability and low modulus, and preparation method and application thereof - Google Patents
Temporary bonding glue with high thermal stability and low modulus, and preparation method and application thereof Download PDFInfo
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- CN112980364A CN112980364A CN202110167123.4A CN202110167123A CN112980364A CN 112980364 A CN112980364 A CN 112980364A CN 202110167123 A CN202110167123 A CN 202110167123A CN 112980364 A CN112980364 A CN 112980364A
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- 239000003292 glue Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000853 adhesive Substances 0.000 claims abstract description 56
- 230000001070 adhesive effect Effects 0.000 claims abstract description 56
- 239000011521 glass Substances 0.000 claims description 53
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 14
- 150000003384 small molecules Chemical class 0.000 claims description 11
- 239000012790 adhesive layer Substances 0.000 claims description 9
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 229920002866 paraformaldehyde Polymers 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000003929 acidic solution Substances 0.000 claims description 3
- GPXCORHXFPYJEH-UHFFFAOYSA-N 3-[[3-aminopropyl(dimethyl)silyl]oxy-dimethylsilyl]propan-1-amine Chemical group NCCC[Si](C)(C)O[Si](C)(C)CCCN GPXCORHXFPYJEH-UHFFFAOYSA-N 0.000 claims description 2
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical group C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 235000012431 wafers Nutrition 0.000 description 17
- 230000004580 weight loss Effects 0.000 description 13
- 239000000463 material Substances 0.000 description 7
- 230000009477 glass transition Effects 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- 238000002791 soaking Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000012545 processing Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000000113 differential scanning calorimetry Methods 0.000 description 4
- 238000002411 thermogravimetry Methods 0.000 description 4
- 230000002123 temporal effect Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012536 packaging technology Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C09J161/22—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/04—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
- C08G12/06—Amines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/04—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
- C08G12/06—Amines
- C08G12/08—Amines aromatic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
- C09J5/06—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving heating of the applied adhesive
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/10—Presence of inorganic materials
- C09J2400/14—Glass
- C09J2400/143—Glass in the substrate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2461/00—Presence of condensation polymers of aldehydes or ketones
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention belongs to the technical field of temporary bonding glue, and particularly relates to a preparation method and application of temporary bonding glue with high thermal stability and low modulus. According to the preparation method, a small amount of flexible molecular chain segments are introduced into the rigid molecular chain segments, so that the modulus of the bonding adhesive is reduced under the condition that the thermal stability is not lost or is less lost, and the bonding adhesive has a good application prospect in the temporary bonding application scene of ultrathin and fragile objects.
Description
Technical Field
The invention belongs to the technical field of temporary bonding glue, and particularly relates to temporary bonding glue with high thermal stability and low modulus as well as a preparation method and application thereof.
Background
In recent years, in order to meet the rapid development of industries such as computer, communication, automobile, aerospace, and electronic industries, microelectronic packaging technology is faced with high requirements such as smaller, thinner, lighter, multifunctional, and low cost. The semiconductor industry often requires thinning device wafers to below 100um with vertical interconnects between the thin wafers to achieve high density stack packaging. However, when the thickness of the wafer is less than 100um and there is no support, the wafer is easily warped and broken during processing. At this point, the device wafer and the thicker carrier need to be bonded together with a temporary adhesive, and the carrier provides sufficient mechanical support for the thin wafer to complete wafer thinning and subsequent backside processing.
Common temporary bonding glue includes thermoplastic temporary bonding glue, laser degradable temporary bonding glue, and chemically degradable temporary bonding glue. However, these materials suffer from poor thermal stability, high modulus of the material, and difficulty in degradation and cleaning. Poor thermal stability can cause blistering during processing, resulting in large cracks in the wafer. High material modulus can lead to wafer warpage. The difficulty in degradation and cleaning can cause the residual glue on the wafer to affect the subsequent process.
Currently, the BREWER HT1010 softening point of the available adhesives is only 180 ℃ (Lee A, Su J, McCutcheon J, et al. optimization of temporal bonding high-resolution adhesives to a thermal in-process bonding [ C ]// processes of IEEE 14th Electronics Packaging Technology Conference,2012: 322. 325.), 3MWSS heat resistant adhesives can reach about 220 ℃, but bonding requires a protective film with bonding capability, and thin wafers finally need to be separated from the protective film, reducing the bonding efficiency (correlation J. in wafer bonding-simulation of the temporal bonding of [ C ]/processing of IEEE 3. I. 2009: 1. System). SAMPLE-A as an adhesive developed by Shuainianxing et al has a heat-resistant temperature of over 300 ℃ and bonding strength of 21MPA, but debonding requires thermal slippage at a high temperature of over 235 ℃, and the destruction rate of a wafer is high (GB/T7714 Shuainianxing, Zhangguo Ping, Dunli wave, et al, temporary bonding glue [ J ] integration technology for thin wafer processing, 2014(6): 102-. The novel temporary adhesive debonding developed by Deng et al required 10H (Deng L, Fang H, Shuai X, et al. preparation of reversible thermosets and the present application in temporal adhesive for the use of a in water handling [ J ]. Proceedings-Electronic Components and Technology Conference,2015,2015: 1197. 1201.).
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the invention aims to provide a preparation method of a temporary bonding adhesive with high thermal stability and low modulus, which has the advantages of simple process and low cost, and can prepare the temporary bonding adhesive with high thermal stability, low modulus and easy degradability.
The second purpose of the invention is to provide a temporary adhesive obtained by the preparation method.
A third object of the invention is to provide the use of such a temporary adhesive.
The primary purpose of the invention is realized by the following technical scheme:
a preparation method of temporary bonding glue with high thermal stability and low modulus comprises the following steps: according to the mass ratio of the curing agent, the hard segment micromolecules, the soft segment micromolecules and the N-methylpyrrolidone (NMP) of 5: 0.8-0.9: 0.1-0.2: 0.3, preparing raw materials, dissolving a curing agent, hard-segment small molecules and soft-segment small molecules in N-methylpyrrolidone (NMP) at 50-100 ℃, stirring and mixing to dissolve the raw materials to form the temporary adhesive.
Preferably, the curing agent is paraformaldehyde ((CH)2O)n)。
Preferably, the hard segment micromolecules are molecules containing benzene ring rigid structures, and can play a role in high thermal stability of the temporary adhesive glue.
Preferably, the hard segment small molecule is 4,4' -diaminodiphenyl ether (ODA).
Preferably, the soft segment small molecule is a molecule containing siloxane or/and alkyl structure, and plays a role in reducing the modulus of the temporary adhesive glue.
Preferably, the soft segment small molecule is 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane (BATDS).
The second purpose of the invention is realized by the following technical scheme:
a temporary bonding paste having high thermal stability and low modulus prepared by the preparation method of any one of the above.
The third purpose of the invention is realized by the following technical scheme:
the application of a temporary adhesive with high thermal stability and low modulus.
Preferably, the temporary bonding glue with high thermal stability and low modulus is applied in a bonding process.
Specifically, the prepared temporary bonding glue with high thermal stability and low modulus is injected to the surface of a glass sheet by a syringe, then another glass sheet is attached to the surface, and then the glass sheet is heated according to the following steps: heating at 100 ℃ for 0.5h and heating at 200-250 ℃ for 1h, and finally curing to obtain an adhesive layer to firmly adhere the two pieces of glass.
Preferably, the temperature for forming the adhesive layer is 200 ℃.
Preferably, the temporary bonding glue with high thermal stability and low modulus is applied in a debonding process.
Specifically, after the glass sheets bonded by the temporary bonding glue are placed in an acid solution to be soaked for 6 hours at the shortest time, the two glass sheets can be easily separated.
Preferably, the acidic solution can be sulfuric acid or hydrochloric acid, and the concentration is 0.5-2 mol/L.
Compared with the prior art, the invention has the advantages that:
the preparation method of the adhesive is simple, and the raw materials are easy to obtain; the prepared adhesive has the following capabilities of high heat resistance temperature, low modulus and easy degradation: the higher heat-resistant temperature can avoid the generation of bubbles in the manufacturing process, thereby avoiding the generation of cracks on the wafer; the lower modulus can avoid the warping of the wafer; the bonding glue is easy to degrade, so that the wafer can be easily separated from the glass substrate, and low molecules and oligomers generated after degradation can be easily cleaned to avoid residual glue; the method realizes the reliability and low cost of bonding and debonding, and has the advantages of simple operation and low cost.
Drawings
Fig. 1 is a flowchart of an embodiment of the present invention in embodiment 1:
in the figure (a), a layer of glass sheet is covered after the solution is dripped on the glass sheet, and heating and curing are carried out; panel (b) after curing, the two sheets of glass are tightly bonded and cannot be separated by hand; figure (c) the glass sheet is soaked in 0.5mol/L sulfuric acid solution; after soaking, the two glass sheets can be easily separated by hand.
Fig. 2 is a TG data diagram of the adhesive paste added with hard segments and soft segments of different ratios in examples 1 to 4 of the present invention:
wherein S0 is the thermal weight loss data of the adhesive glue containing only hard segment and no soft segment; s1 is the thermal weight loss data of the adhesive with the molar ratio of the hard segment to the soft segment being 9: 1; s2 is the thermal weight loss data of the adhesive with the molar ratio of the hard segment to the soft segment being 8: 2; s3 is the thermal weight loss data of the adhesive with the molar ratio of the hard segment to the soft segment being 6: 4.
FIG. 3 is a DSC data chart of the adhesive glue with different proportions of hard segment and soft segment added in examples 1 to 4 of the present invention:
wherein S0 is DSC data of the adhesive glue containing only hard segments and no soft segments; s1 is DSC data of the adhesive with the molar ratio of the hard segment to the soft segment being 9: 1; s2 is DSC data of the adhesive cement with the molar ratio of the hard segment to the soft segment being 8: 2; s3 is DSC data for a bond paste having a 6:4 molar ratio of hard segments to soft segments.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
(1) Weighing 0.150g of paraformaldehyde, 0.2g of ODA and 0g of BATDS, dissolving the two in 3.0mL of NMP, and mixing and stirring at 100 ℃ for about 15min to fully dissolve the monomers to generate a temporary adhesive; )
(2) Injecting the temporary bonding glue solution obtained in the step (1) to the surface of a glass sheet with the thickness of 30 multiplied by 30cm by using a syringe, then attaching another glass sheet to the surface, and then heating the glass sheet according to the following steps: heating at 100 ℃ for 0.5h and at 200 ℃ for 1h, and finally curing to obtain an adhesive layer to firmly adhere the two pieces of glass;
(3) after the glass sheets bonded by the temporary bonding glue are soaked in a 0.5mol/mL sulfuric acid solution for 48 hours, the two glass sheets can be easily separated, as shown in FIG. 1.
The TG analysis of the adhesive showed that the adhesive had a temperature of 201.1% weight loss and a temperature of 263.0% weight loss of 1% weight loss, as shown in S0 in fig. 2. DSC analysis of the adhesive showed that the adhesive had no significant glass transition and the material was significantly brittle as shown in S0 in fig. 3.
Example 2
(1) Weighing 0.150g of paraformaldehyde, 0.18g of ODA and 0.025g of BATDS, dissolving the three in 3.0mL of NMP, and mixing and stirring at 100 ℃ for about 15min to fully dissolve the monomers to generate a temporary adhesive;
(2) injecting the temporary bonding glue solution obtained in the step (1) to the surface of a glass sheet with the thickness of 30 multiplied by 30cm by using a syringe, then attaching another glass sheet to the surface, and then heating the glass sheet according to the following steps: heating at 100 ℃ for 0.5h and at 200 ℃ for 1h, and finally curing to obtain an adhesive layer to firmly adhere the two pieces of glass;
(3) after the glass sheets bonded by the temporary bonding glue are placed into a 2mol/mL sulfuric acid solution for soaking for 6 hours, the two glass sheets can be easily separated.
TG analysis of the adhesive showed that the adhesive had a temperature of 231.7% weight loss and a temperature of 277.0% weight loss of 1%, as shown in S1 in fig. 2. DSC analysis of the adhesive shows that the glass transition temperature of the adhesive is 118.4 ℃ as shown in S1 in FIG. 3, and the material has good toughness.
Example 3
(1) Weighing 0.150g of paraformaldehyde, 0.16g of ODA and 0.05g of BATDS, dissolving the three in 3.0mL of NMP, and mixing and stirring at 100 ℃ for about 15min to fully dissolve the monomers to generate a temporary adhesive;
(2) injecting the temporary bonding glue solution obtained in the step (1) to the surface of a glass sheet with the thickness of 30 multiplied by 30cm by using a syringe, then attaching another glass sheet to the surface, and then heating the glass sheet according to the following steps: heating at 100 ℃ for 0.5h and at 200 ℃ for 1h, and finally curing to obtain an adhesive layer to firmly adhere the two pieces of glass;
(3) after the glass sheets bonded by the temporary bonding glue are placed into a 2mol/mL sulfuric acid solution for soaking for 8 hours, the two glass sheets can be easily separated.
TG analysis of the adhesive showed that the adhesive had a 1% weight loss temperature of 223.0 ℃ and a 5% weight loss temperature of 271.5 ℃ as shown in FIG. 2S 2. DSC analysis of the adhesive showed that the glass transition temperature of the adhesive was 94.3 ℃ as shown in FIG. 3S2, and the material had good toughness.
Example 4
(1) Weighing 0.150g of paraformaldehyde, 0.16g of ODA and 0.05g of BATDS, dissolving the three in 3.0mL of NMP, and mixing and stirring at 100 ℃ for about 15min to fully dissolve the monomers to generate a temporary adhesive;
(2) injecting the temporary bonding glue solution obtained in the step (1) to the surface of a glass sheet with the thickness of 30 multiplied by 30cm by using a syringe, then attaching another glass sheet to the surface, and then heating the glass sheet according to the following steps: heating at 100 ℃ for 0.5h and at 200 ℃ for 1h, and finally curing to obtain an adhesive layer to firmly adhere the two pieces of glass;
(3) after the glass sheets bonded by the temporary bonding glue are placed into a 2mol/mL sulfuric acid solution for soaking for 8 hours, the two glass sheets can be easily separated.
TG analysis of the adhesive showed that the adhesive had a temperature of 217.3% weight loss and a temperature of 267.2% weight loss of 1% as shown in S3 in fig. 2. DSC analysis of the adhesive shows that the glass transition temperature of the adhesive is 61.0 ℃ as shown in S3 in FIG. 3, and the material has good toughness.
Example 5
(1) Weighing 0.150g of paraformaldehyde, 0.18g of ODA and 0.025g of BATDS, dissolving the three in 3.0mL of NMP, and mixing and stirring at 100 ℃ for about 15min to fully dissolve the monomers to generate a temporary adhesive;
(2) injecting the temporary bonding glue solution obtained in the step (1) to the surface of a glass sheet with the thickness of 30 multiplied by 30cm by using a syringe, then attaching another glass sheet to the surface, and then heating the glass sheet according to the following steps: heating at 100 ℃ for 0.5h and at 220 ℃ for 1h, and finally curing to obtain an adhesive layer to firmly adhere the two pieces of glass;
(3) after the glass sheets bonded by the temporary bonding glue are placed into a 2mol/mL sulfuric acid solution for soaking for 8 hours, the two glass sheets can be easily separated.
The TG and glass transition temperature of the adhesive was comparable to that of example 2.
Example 6
(1) Weighing 0.150g of paraformaldehyde, 0.18g of ODA and 0.025g of BATDS, dissolving the three in 3.0mL of NMP, and mixing and stirring at 100 ℃ for about 15min to fully dissolve the monomers to generate a temporary adhesive;
(2) injecting the temporary bonding glue solution obtained in the step (1) to the surface of a glass sheet with the thickness of 30 multiplied by 30cm by using a syringe, then attaching another glass sheet to the surface, and then heating the glass sheet according to the following steps: heating at 100 ℃ for 0.5h and at 250 ℃ for 1h, and finally curing to obtain an adhesive layer to firmly adhere the two pieces of glass;
(3) after the glass sheets bonded by the temporary bonding glue are placed into a 2mol/mL sulfuric acid solution for soaking for 8 hours, the two glass sheets can be easily separated.
The TG and glass transition temperature of the adhesive was comparable to that of example 2.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of temporary bonding glue with high thermal stability and low modulus is characterized by comprising the following steps: according to the mass ratio of the curing agent, the hard segment micromolecules, the soft segment micromolecules and the N-methylpyrrolidone (NMP) of 5: 0.8-0.9: 0.1-0.2: 0.3, preparing raw materials, dissolving a curing agent, hard-segment small molecules and soft-segment small molecules in N-methylpyrrolidone (NMP) at 50-100 ℃, stirring and mixing to dissolve the raw materials to form the temporary adhesive.
2. A method for preparing a temporary bonding paste having high thermal stability and low modulus as claimed in claim 1, wherein the curing agent is paraformaldehyde.
3. A method for preparing a temporary bonding paste with high thermal stability and low modulus as claimed in claim 1, wherein said hard segment small molecule is a molecule having a rigid structure of benzene ring.
4. A method for preparing a temporary bonding paste having high thermal stability and low modulus as claimed in claim 3, wherein the hard segment small molecule is 4,4' -diaminodiphenyl ether.
5. A method for preparing a temporary bonding paste having high thermal stability and low modulus as claimed in claim 1, wherein said soft segment small molecule is a molecule containing siloxane or/and alkyl structure.
6. A method of preparing a temporary bonding paste having high thermal stability and low modulus as claimed in claim 5, wherein said soft segment small molecule is 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane.
7. A temporary bonding paste having high thermal stability and low modulus prepared by the preparation method according to any one of claims 1 to 6.
8. Use of a temporary bonding glue with high thermal stability and low modulus according to claim 7 in a bonding process, characterized by the specific steps of: the prepared temporary bonding glue with high thermal stability and low modulus is injected to the surface of a glass sheet by a syringe, then another glass sheet is attached to the surface, and then the glass sheet is heated according to the following steps: heating at 100 ℃ for 0.5h and heating at 200-250 ℃ for 1h, and finally curing to obtain an adhesive layer to firmly adhere the two pieces of glass.
9. Use of a temporary bonding adhesive with high thermal stability and low modulus according to claim 7 in a debonding process, wherein the two glass sheets bonded by the temporary bonding adhesive can be easily separated after being soaked in an acidic solution for 6 hours.
10. The use of a temporary bonding adhesive with high thermal stability and low modulus according to claim 9 in a debonding process, wherein the acidic solution is a sulfuric acid solution or a hydrochloric acid solution with a concentration of 0.5-2 mol/L.
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| JP2005120269A (en) * | 2003-10-17 | 2005-05-12 | Shin Etsu Chem Co Ltd | Adhesive composition, adhesive film, and adhesive tape for dicing and die bonding |
| CN102925088A (en) * | 2011-08-10 | 2013-02-13 | 烟台德邦科技有限公司 | Solar crystalline silicon wafer temporary adhesive and its preparation method |
| CN104559852A (en) * | 2014-12-31 | 2015-04-29 | 深圳先进技术研究院 | Temporary bonding adhesive for processing thin wafer and preparation method of temporary bonding adhesive |
| CN104804682A (en) * | 2015-04-16 | 2015-07-29 | 深圳先进技术研究院 | Temporary bonding glue for wafer backgrinding, preparation method of temporary bonding glue and bonding and de-bonding methods |
| CN105255425A (en) * | 2015-11-19 | 2016-01-20 | 杭州得力科技有限公司 | Bi-component epoxy adhesive for temporary adhesion as well as preparation method and application of bi-component epoxy adhesive |
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