CN112602172A - Adhesive tape for dicing and method for manufacturing semiconductor chip - Google Patents
Adhesive tape for dicing and method for manufacturing semiconductor chip Download PDFInfo
- Publication number
- CN112602172A CN112602172A CN201980055642.2A CN201980055642A CN112602172A CN 112602172 A CN112602172 A CN 112602172A CN 201980055642 A CN201980055642 A CN 201980055642A CN 112602172 A CN112602172 A CN 112602172A
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- China
- Prior art keywords
- adhesive
- silicone
- adhesive tape
- dicing
- mass
- Prior art date
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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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
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Adhesive Tapes (AREA)
- Dicing (AREA)
Abstract
An adhesive tape for dicing, which comprises a base material and a silicone adhesive layer laminated on the base material, and is used when a semiconductor material having a plurality of semiconductor elements covered with a coating material is divided into a plurality of semiconductor chips, wherein the silicone adhesive layer comprises an addition reaction type silicone adhesive as a main agent, and contains a photosensitive platinum (Pt) catalyst and a crosslinking agent for the addition reaction type silicone adhesive, the mass ratio of a silicone rubber material to a silicone resin is in the range of 35/65 to 50/50, and the content ratio of a silicone rubber material having an alkenyl group in the total mass of the silicone rubber material and the silicone resin is in the range of 35 mass% to 50 mass%.
Description
Technical Field
The present invention relates to an adhesive tape for dicing used for dicing a semiconductor material as a semiconductor chip material, and a method for manufacturing a semiconductor chip using the adhesive tape for dicing.
Background
Conventionally, as an adhesive tape for dicing for producing a semiconductor chip having an LED (Light Emitting Diode) or the like, an adhesive tape having an adhesive layer made of an acrylic resin has been known (see patent document 1).
Further, as an adhesive tape for dicing for producing a semiconductor chip having an LED or the like, an adhesive tape having an adhesive layer made of a silicone resin is known (see patent documents 2 and 3).
Further, as a method for manufacturing a semiconductor chip using an adhesive tape for dicing, the following method is known: an adhesive tape is attached to a substrate side of a semiconductor element substrate having a plurality of semiconductor elements formed on a substrate, and the semiconductor element substrate is cut by a dicing saw (see patent document 4).
Documents of the prior art
Patent document
Patent document 1: japanese patent laid-open publication No. 2013-38408
Patent document 2: japanese patent laid-open publication No. 2015-050216
Patent document 3: japanese patent laid-open publication No. 2016-
Patent document 4: japanese patent laid-open publication No. 2005-93503
Disclosure of Invention
Problems to be solved by the invention
In recent years, as a method for manufacturing a semiconductor chip singulated by dicing, the following techniques have been proposed: a technique of attaching an adhesive tape to a semiconductor material in which a plurality of semiconductor elements are coated with a coating material such as a sealing resin or a phosphor, and dicing the semiconductor material; a technique corresponding to a so-called wafer-level CSP (chip scale package) process.
In the case where the adhesive tape is applied to a semiconductor material in which a semiconductor element is covered with a coating material, the adhesive layer in the adhesive tape may have insufficient adhesive strength due to the composition of the adhesive layer and the material of the coating material, and the semiconductor chips singulated by dicing may be scattered. Further, if the ball tack and the adhesive force of the adhesive layer are designed to be high in order to suppress the scattering of the semiconductor chip, so-called adhesive residue may occur in which the adhesive remains in the semiconductor chip in an adhered state when the obtained semiconductor chip is peeled off from the adhesive tape.
The invention aims to provide a dicing adhesive tape which has good adhesive force and adhesive force to a semiconductor material having a plurality of semiconductor elements covered with a coating material and suppresses adhesive residue to the semiconductor chip when peeling off the semiconductor chip singulated by dicing, and a semiconductor chip manufacturing method using the dicing adhesive tape.
Means for solving the problems
In view of the above-described object, the present inventors have intensively studied the adhesive layer of the adhesive tape for dicing, and as a result, have found that: the present inventors have found that if a photosensitive platinum (Pt) catalyst is added to a specific adhesive containing at least an addition reaction type silicone adhesive and a crosslinking agent for the addition reaction type silicone adhesive, the adhesive layer has a good adhesive force to a semiconductor material having a plurality of semiconductor elements coated with a coating material, and can suppress adhesive residue on a semiconductor chip when the semiconductor chip singulated by dicing is peeled off, and thus the present invention has been completed.
Namely, it was found that: by configuring the adhesive layer of the dicing adhesive tape as described above, when a semiconductor material having a plurality of semiconductor elements covered with a coating material is divided into a plurality of semiconductor chips, the semiconductor chips singulated during dicing can be suppressed from scattering due to good adhesive force and adhesive force. On the other hand, when the semiconductor chip singulated by dicing is peeled off from the dicing adhesive tape, the photosensitive platinum (Pt) catalyst in the adhesive is activated by irradiating the adhesive layer with light such as ultraviolet rays, and the crosslinking reaction between the addition reaction type silicone adhesive and the crosslinking agent for the addition reaction type silicone adhesive is promoted, so that the cohesive force of the adhesive becomes larger than that before the light irradiation. As a result, the adhesive force of the adhesive layer is appropriately reduced, and the failure mode in the retention test is "interfacial peeling" or "no drop" in the retention test. It is thus found that the semiconductor chip can be picked up from the dicing adhesive tape well and that the adhesive residue on the semiconductor chip can be suppressed.
The adhesive tape for dicing of the present invention is characterized by comprising a base material and a silicone adhesive layer laminated on the base material, and is used when a semiconductor material having a plurality of semiconductor elements covered with a coating material is divided into a plurality of semiconductor chips, wherein the silicone adhesive layer comprises an addition reaction type silicone adhesive as a main agent, and contains a photosensitive platinum (Pt) catalyst and a crosslinking agent for the addition reaction type silicone adhesive, the mass ratio (Gw)/(Rw) of the total mass (Gw) of a silicone rubber (G) contained in the silicone adhesive layer to the total mass (Rw) of a silicone resin (R) is in the range of 35/65 to 50/50, and the content ratio of a silicone rubber (G1) having an alkenyl group in the total mass of the silicone rubber (G) and the silicone resin (R) is 35 mass% or more and 50 mass% or more % satisfies all of the following conditions (a) to (c) in the adhesive properties according to JIS Z0237 (2009).
(a) The adhesion to a BA-SUS test plate before light irradiation was 2.4N/10mm or more and 5.5N/10mm or less.
(b) Regarding the ball number in the inclined ball viscosity test (inclination angle 30 °, temperature 23 ℃, relative humidity 50% RH), when the ball number before light irradiation is BN0 and the ball number after light irradiation is BN1, the relationship BN0 > BN1 is obtained.
(c) In the retention test (temperature 40 ℃, relative humidity 33% RH, standing time 5000 minutes) after the light irradiation, the phenomenon of breakage at the time of dropping means that the silicone adhesive layer peels off from the interface with the BA-SUS test plate or does not drop in the retention test.
Here, the dicing adhesive tape may be characterized in that the semiconductor material in which the plurality of semiconductor elements are sealed with the coating material made of silicone resin is used by being stuck from the coating material side.
From another viewpoint, the adhesive tape for dicing of the present invention is an adhesive tape for dicing used for dividing a semiconductor material having a plurality of semiconductor elements covered with a coating material into a plurality of semiconductor chips, the adhesive tape for dicing comprising a base material and a silicone adhesive layer laminated on the base material, wherein the silicone adhesive layer comprises a mixture of an addition reaction type silicone adhesive and a peroxide curing type silicone adhesive as a main component, and contains a photosensitive platinum (Pt) catalyst and a crosslinking agent for the addition reaction type silicone adhesive, and a mass ratio (Gw)/(Rw) of a total mass (Gw) of a silicone gum (G) contained in the silicone adhesive layer to a total mass (Rw) of a silicone resin (R) is in a range of 40/60 to 56/44, the content ratio of the silicone rubber compound (G1) having an alkenyl group in the total mass of the silicone rubber compound (G) and the silicone resin (R) is in the range of 14 mass% or more and 42 mass% or less, and all of the following conditions (a) to (c) are satisfied in the adhesive properties according to JIS Z0237 (2009).
(a) The adhesion to a BA-SUS test plate before light irradiation was 2.4N/10mm or more and 5.5N/10mm or less.
(b) Regarding the ball number in the inclined ball viscosity test (inclination angle 30 °, temperature 23 ℃, relative humidity 50% RH), when the ball number before light irradiation is BN0 and the ball number after light irradiation is BN1, the relationship BN0 > BN1 is obtained.
(c) In the retention test (temperature 40 ℃, relative humidity 33% RH, standing time 5000 minutes) after the light irradiation, the phenomenon of breakage at the time of dropping means that the silicone adhesive layer peels off from the interface with the BA-SUS test plate or does not drop in the retention test.
Here, the dicing adhesive tape may be characterized in that the semiconductor material in which the plurality of semiconductor elements are sealed with the coating material made of silicone resin is used by being stuck from the coating material side.
The silicone adhesive layer may further include an initiator composed of a peroxide.
From another viewpoint, a method for manufacturing a semiconductor chip according to the present invention is a method for manufacturing a semiconductor chip including the steps of: a bonding step of bonding the dicing adhesive tape to a semiconductor element substrate having formed thereon a plurality of the semiconductor elements sealed with a sealing resin made of a silicone resin from the sealing resin side; a cutting step of cutting the semiconductor element substrate to which the adhesive tape for dicing is attached into a plurality of semiconductor chips; an irradiation step of irradiating the dicing adhesive tape of the semiconductor element substrate with light; and a peeling step of peeling the dicing adhesive tape from the plurality of semiconductor chips.
Effects of the invention
According to the present invention, it is possible to provide an adhesive tape for dicing which has excellent adhesive force and adhesive force in a stage before light irradiation to a semiconductor material in which a plurality of semiconductor elements are covered with a covering material, has excellent pickup properties of semiconductor chips when the semiconductor chips singulated by dicing are peeled off after light irradiation, and suppresses adhesive residue on the semiconductor chips, and a method for manufacturing a semiconductor chip using the adhesive tape for dicing.
Drawings
Fig. 1 is a view showing an example of a structure to which the adhesive tape for dicing of the present embodiment is applied.
Fig. 2(a) to (e) are diagrams showing a method for manufacturing a semiconductor chip using the adhesive tape of the present embodiment.
FIG. 3 is a schematic diagram showing the relationship between the crosslink density of an addition reaction type silicone adhesive in an adhesive layer and the result of a holding force test (falling time) of an adhesive tape.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.
[ construction of adhesive tape ]
Fig. 1 is a diagram showing an example of a structure to which an adhesive tape 1 for dicing (hereinafter, simply referred to as an adhesive tape 1) of the present embodiment is applied. The adhesive tape 1 of the present embodiment is used for dicing a semiconductor material as a raw material of a semiconductor chip in a manufacturing process of the semiconductor chip having a semiconductor element such as an LED (Light emitting diode) or a power semiconductor.
As shown in fig. 1, the adhesive tape 1 has a structure in which an adhesive layer 3, which is an example of a silicone adhesive layer, is laminated on a substrate 2.
Although not shown, the adhesive tape 1 may further include an anchor coat layer (anchor coat layer) between the base material 2 and the adhesive layer 3 as necessary to improve the adhesion between the base material 2 and the adhesive layer 3. Further, the surface of the substrate 2 (the surface opposite to the surface facing the adhesive layer 3) may be subjected to a surface treatment. Further, a release liner may be provided on the surface of the adhesive layer 3 (the surface opposite to the surface facing the substrate 2).
< substrate >
The base material 2 of the present embodiment is made of a material that transmits light such as ultraviolet rays. The material of the base material 2 is not particularly limited as long as it can transmit light such as ultraviolet rays, and for example, plastic or the like through which light such as ultraviolet rays can transmit can be used. Here, the term "light-transmittable" of ultraviolet rays or the like does not mean that the transmittance of light such as ultraviolet rays is 100%, and it is sufficient that at least light of a degree that promotes the addition reaction of the addition reaction type silicone adhesive and the crosslinking agent in the adhesive layer 3 by the photosensitive platinum (Pt) catalyst described later is transmittable.
As a material of the substrate 2, specifically, a resin film such as polyethylene terephthalate, polyethylene naphthalate, polyphenylene sulfide, biaxially stretched polypropylene, aliphatic polyimide (transparent polyimide), polycycloolefin, fluorine-based resin, polyolefin resin, or the like can be used. In addition, depending on the application, for example, a composite film obtained by laminating a polyethylene terephthalate and a polyolefin resin film, a composite film obtained by further laminating these composite films with a resin film, a resin film formed into a plurality of layers by coextrusion, or the like may be used for the substrate 2.
Among them, a material containing polyethylene terephthalate as a main component is preferably used as the substrate 2.
< adhesive layer >
The adhesive layer 3 of the present embodiment includes a curable silicone adhesive. Specifically, the adhesive layer 3 contains an addition reaction type silicone adhesive as a curing type silicone adhesive. The adhesive layer 3 may contain a peroxide-curable silicone adhesive as a curable silicone adhesive in addition to an addition-reactive silicone adhesive. In general, both the addition reaction type silicone adhesive and the peroxide curing type silicone adhesive include a silicone gum (G) composed of an organopolysiloxane and a silicone resin (R) composed of an organopolysiloxane.
Hereinafter, each component constituting the adhesive layer 3 will be described in detail with reference to the adhesive layer 3 including an addition reaction type silicone adhesive as a curing type silicone adhesive as a first embodiment, and the adhesive layer 3 including an addition reaction type silicone adhesive and a peroxide curing type silicone adhesive as a second embodiment.
< adhesive layer of the first embodiment >
The adhesive layer 3 of the first embodiment includes an addition-reaction-type silicone adhesive and a crosslinking agent as an example of a curing agent for crosslinking the addition-reaction-type silicone adhesive. The adhesive agent layer 3 of the first embodiment contains a photosensitive platinum (Pt) catalyst that promotes the reaction between the addition reaction type silicone adhesive and the crosslinking agent by irradiation with light such as ultraviolet light. The adhesive layer 3 of the first embodiment does not contain a peroxide-curable silicone adhesive.
Further, the adhesive agent layer 3 of the first embodiment may further contain other additives such as a reinforcing filler, a cohesive force improving agent, and a colorant, as necessary.
(addition reaction type Silicone adhesive)
Conventionally known adhesives can be used as the addition reaction type silicone adhesive, but in general, the adhesive is an adhesive containing a silicone gum (G1) composed of an organopolysiloxane such as polydimethylsiloxane containing at least 2 alkenyl groups to which silicon atoms are bonded in an average 1 molecule, and a silicone resin (R1) composed of an organopolysiloxane such as polydimethylsiloxane. Here, the silicone resin (R1) composed of an organopolysiloxane such as polydimethylsiloxane does not contain an alkenyl group to which a silicon atom is bonded.
The silicone gum (G1) composed of an organopolysiloxane such as polydimethylsiloxane having at least 2 alkenyl groups to which silicon atoms are bonded in an average of 1 molecule and the silicone resin (R1) composed of an organopolysiloxane such as polydimethylsiloxane, which are contained in the addition reaction type silicone adhesive, will be described in further detail below.
In the following description, a silicone gum (G1) composed of an organopolysiloxane such as polydimethylsiloxane containing at least 2 alkenyl groups bonded to silicon atoms in an average of 1 molecule may be expressed as a silicone gum (G1) composed of an organopolysiloxane such as polydimethylsiloxane containing alkenyl groups bonded to silicon atoms or as a silicone gum (G1) having only alkenyl groups.
[ Silicone rubber (G1) comprising organopolysiloxane such as polydimethylsiloxane having silicon atom-bonded alkenyl group ]
The silicone gum (G1) composed of an organopolysiloxane such as polydimethylsiloxane containing alkenyl groups to which silicon atoms are bonded in the present embodiment is not particularly limited as long as it is a silicone gum used in an addition reaction type silicone-based adhesive, that is, a silicone gum containing at least 2 alkenyl groups to which silicon atoms are bonded in an average of 1 molecule. Examples of the molecular structure of the organopolysiloxane such as polydimethylsiloxane containing an alkenyl group to which a silicon atom is bonded include a linear structure in which a main chain portion is composed of diorganosiloxane repeating units, a structure in which a part of the molecular structure includes a branched chain, a branched chain structure, or a cyclic structure. Among them, organopolysiloxanes having a linear structure are preferable in terms of mechanical strength and physical properties of the adhesive after irradiation with light such as ultraviolet rays.
The silicone gum (G1) composed of an organopolysiloxane containing alkenyl groups to which silicon atoms are bonded may be oily or raw gum-like, preferably raw gum-like.
When the silicone rubber (G1) is oily, the viscosity of the silicone rubber (G1) composed of the organopolysiloxane is preferably 1,000mPa · s or more at 25 ℃. If the viscosity is less than 1000mPa · s, the adhesive may not exhibit desired adhesive properties before and after light irradiation, and the adhesion between the adhesive layer 3 and the substrate 2 may be deteriorated.
In the case of a raw gum, the viscosity of a silicone gum (G1) composed of an organopolysiloxane when dissolved in toluene at a concentration of 30 mass% is preferably 100,000mPa · s or less at 25 ℃. If the viscosity exceeds 100,000 mPas, stirring may become difficult in preparing the adhesive composition.
The viscosity can be measured using a BM type rotational viscometer.
Examples of the silicone gum (G1) composed of an organopolysiloxane containing alkenyl groups to which silicon atoms are bonded include, but are not limited to, those represented by the following general formula (1) or general formula (2).
[ solution 1]
R1 (3-a)XaSiO-(R1XSiO)m-(R1 2SiO)n-SiR1 (3-a)XaGeneral formula (1)
[ solution 2]
R1 2(OH)SiO-(R1XSiO)m+2-(R1 2SiO)n-SiR1 2(OH) general formula (2)
Here, in the above general formulae (1) and (2), R1Independently of one another, a monovalent hydrocarbon group having no aliphatic unsaturated bond, and X is an organic group having an alkenyl group. a is an integer of 0 to 3, m is an integer of 0 or more, and n is an integer of 100 or more, but a and m are not 0 at the same time. m + n is a value at which the viscosity of the organopolysiloxane at 25 ℃ is 1,000 mPas or more.
As R1The monovalent hydrocarbon group having no aliphatic unsaturated bond and having 1 to 10 carbon atoms, preferably 1 to 7 carbon atoms, is preferable. Examples thereof include alkyl groups such as methyl, ethyl, propyl, and butyl; cycloalkyl groups such as cyclohexyl; and aryl groups such as phenyl and tolyl, and methyl and phenyl are particularly preferable.
X is preferably an organic group containing an alkenyl group having 2 to 10 carbon atoms. Examples thereof include vinyl, allyl, hexenyl, octenyl, acryloylpropyl, acryloylmethyl, methacryloylpropyl, acryloyloxypropyl, acryloyloxymethyl, methacryloyloxypropyl, methacryloyloxymethyl, cyclohexenylethyl, and vinyloxypropyl groups. Among them, lower alkenyl groups such as vinyl and allyl are preferable, and vinyl is particularly preferable from the industrial viewpoint. The bonding position of the alkenyl group is not particularly limited, and may be a molecular chain end, a molecular chain side chain, or both the molecular chain end and the molecular chain side chain.
The number of alkenyl groups varies within an appropriate range depending on the content of the silicone resin (R1) composed of an organopolysiloxane such as polydimethylsiloxane contained in the addition reaction type silicone adhesive, the addition amount of the crosslinking agent, and other additive components, and therefore, for example, the range of 0.1 to 3.0 groups is generally preferable to 100 organic groups of the organopolysiloxane. The molecular weight is adjusted within the range of the ratio so as to fall within the above viscosity range, and preferably adjusted so that the number of the above alkenyl groups in the molecule of the organopolysiloxane 1 is at least 2 on average. If the number of alkenyl groups is less than 0.1 relative to 100 organic groups of the organopolysiloxane, the adhesive is less likely to be cured when the adhesive tape 1 is irradiated with light, and the cohesive force is less likely to be increased. In this case, a desired lowering of the adhesive force and a failure mode in the holding force test cannot be obtained, and when the adhesive tape 1 is used for dicing of a semiconductor element substrate or the like and the obtained semiconductor chip or the like is peeled from the adhesive tape 1, there is a risk that the pickup property of the singulated semiconductor chip is deteriorated and adhesive residue is likely to occur on the semiconductor chip or the like. On the other hand, if the number of alkenyl groups exceeds 3.0 relative to 100 organic groups of the organopolysiloxane, in the case where a release liner subjected to release treatment with fluoroalkyl-modified silicone is provided in the adhesive tape 1, there is a possibility that the release force of the release liner with respect to the adhesive layer 3 becomes large.
[ Silicone resin (R1) comprising organopolysiloxane such as polydimethylsiloxane ]
The silicone resin (R1) composed of an organopolysiloxane such as polydimethylsiloxane of the present embodiment has R2 3SiO0.5Units (M units) and SiO2The organopolysiloxane of units (Q units) is called a so-called MQ resin. The silicone resin (R1) composed of an organopolysiloxane such as polydimethylsiloxane basically has no alkenyl group in the molecule, and conventionally known resins can be used. R2A monovalent hydrocarbon group having 1 to 10 carbon atoms, and R is1Monovalent hydrocarbon groups are exemplified. The organopolysiloxane is preferably represented by R2 3SiO0.5Unit/SiO2R is contained in such a manner that the molar ratio of the unit is in the range of 0.5 to 1.72 3SiO0.5Unit and SiO2And (4) units. If R is2 3SiO0.5Unit/SiO2When the molar ratio of the unit is less than 0.5, the adhesive force or cohesive force of the obtained adhesive agent layer 3 may decrease. On the other hand, if R2 3SiO0.5Unit/SiO2The molar ratio of the units exceeds 1.7The adhesive force and holding power of the obtained adhesive agent layer 3 may decrease. The organopolysiloxane may have an OH group. In this case, the content of OH groups is preferably 4.0 mass% or less with respect to the total mass of the organopolysiloxane. If the OH group exceeds the above upper limit, the curability of the adhesive may be reduced.
In the present embodiment, in order to set the adhesive force of the adhesive tape 1 to 2.4N/10mm or more and 5.5N/10mm or less, MQ resin is preferably used as the silicone resin (R2) made of organopolysiloxane such as polydimethylsiloxane. However, the silicone resin (R2) comprising an organopolysiloxane such as polydimethylsiloxane may contain R as an impurity in the synthesis of MQ resin2SiO1.5Unit (T unit) and/or R2SiO unit (D unit).
The silicone gum (G1) composed of an organopolysiloxane such as polydimethylsiloxane containing an alkenyl group to which a silicon atom is bonded and the silicone resin (R1) composed of an organopolysiloxane such as polydimethylsiloxane can also be used by simply mixing them. In addition, as the silicone compound (G1) composed of an organopolysiloxane such as polydimethylsiloxane containing alkenyl groups bonded to silicon atoms, when the organopolysiloxane represented by the above general formula (2) is contained, a silicone compound (G1) composed of an organopolysiloxane such as polydimethylsiloxane containing alkenyl groups bonded to silicon atoms and a silicone resin (R1) composed of an organopolysiloxane such as polydimethylsiloxane may be used in the form of a (partial) condensation reaction product obtained by reacting in advance the silicone compound (G1) composed of an organopolysiloxane containing alkenyl groups bonded to silicon atoms and the silicone resin (R1) composed of an organopolysiloxane such as polydimethylsiloxane, as long as the characteristics of the present invention are not impaired.
(the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) contained in the adhesive layer of the first embodiment to the total mass (Rw) of the silicone resin (R), and the content ratio of the silicone gum (G1) having an alkenyl group to the total mass of the silicone gum (G) and the silicone resin (R))
In the silicone adhesive constituting the adhesive layer 3 of the first embodiment, the total mass (Gw) of the silicone gum (G) is equal to the mass (G1w) of the silicone gum (G1) composed of an organopolysiloxane such as polydimethylsiloxane containing an alkenyl group to which a silicon atom is bonded in the addition reaction type silicone adhesive. Similarly, in the silicone adhesive constituting the adhesive layer 3 of the first embodiment, the total mass (Rw) of the silicone resin (R) is equal to the mass (R1w) of the silicone resin (R1) composed of an organopolysiloxane such as polydimethylsiloxane in the addition reaction type silicone adhesive.
The mass ratio (Gw)/(Rw) ((G1 w)/(R1w)) of the total mass (Gw) of the silicone gum (G) contained in the adhesive agent layer 3 of the first embodiment to the total mass (Rw) of the silicone resin (R) is preferably in the range of 35/65 to 50/50.
In this case, the content ratio { (G1w)/((Gw) + (Rw)) } × 100 of the silicone gum (G1) having an alkenyl group in the total mass of the silicone gum (G) and the silicone resin (R) is also preferably in the range of 35% by mass or more and 50% by mass or less, as described above.
If the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) to the total mass (Rw) of the silicone resin (R) contained in the adhesive layer 3 of the first embodiment and the content ratio of the silicone gum (G1) having an alkenyl group in the total mass of the silicone gum (G) and the silicone resin (R) are less than the lower limit of the above range, the adhesive is less likely to be cured when the adhesive tape 1 is irradiated with light, and the cohesive force is less likely to increase. In this case, a desired lowering of the adhesive force and a failure mode in the holding force test cannot be obtained, and when the adhesive tape 1 is used for dicing of a semiconductor element substrate or the like and the obtained semiconductor chip or the like is peeled from the adhesive tape 1, there is a risk that the pickup property of the singulated semiconductor chip is deteriorated and the semiconductor chip or the like is likely to have adhesive residue.
On the other hand, if the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) to the total mass (Rw) of the silicone resin (R) contained in the adhesive layer 3 of the first embodiment and the content ratio of the silicone gum (G1) having an alkenyl group in the total mass of the silicone gum (G) and the silicone resin (R) exceed the upper limit of the above range, the adhesive layer 3 becomes too soft due to the silicone gum (G) component in a state in which the adhesive is not cured before irradiation with light. In this case, when the semiconductor element substrate or the like is diced, the dicing vibration is easily transmitted to the adhesive layer 3, and the amplitude may become large, for example, the semiconductor element substrate may be displaced from the reference position. Further, with this, there is a risk that fragments (fragments) are generated on the singulated semiconductor chips, and there is a risk that size variations occur for each individual semiconductor chip.
In contrast, by setting the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) to the total mass (Rw) of the silicone resin (R) contained in the adhesive layer 3 of the first embodiment and the content ratio of the silicone gum (G1) having an alkenyl group in the total mass of the silicone gum (G) and the silicone resin (R) to the above range, the following effects can be achieved. That is, the adhesive layer 3 in an uncured state before being irradiated with light such as ultraviolet light can be given an appropriate adhesive force and adhesive force so as not to cause scattering of semiconductor chips or the like as cut pieces at the time of dicing. On the other hand, after the light irradiation, the cohesive force is improved by curing the adhesive layer 3, and thus a desired mode of failure in the tack strength reduction and holding power test can be obtained. As a result, after the adhesive tape 1 is used for dicing a semiconductor element substrate or the like, good pickup properties can be achieved when the obtained semiconductor chip or the like is peeled off from the adhesive tape 1, and adhesive residue on the semiconductor chip or the like can be suppressed.
Further, as the addition reaction type silicone adhesive of the present invention, a commercially available addition reaction type silicone adhesive may also be used. Specifically, for example, KR3700, KR3701, X-40-3237-1, X-40-3240, X-40-3291-1, X-40-3229, X-40-3270, X-40-3306 (trade names) available from shin-Etsu chemical Co., Ltd, TSR1512, TSR1516 and XR37-B9204 (trade names) available from Mi-El-Mi-Gain-Tech materials Co., Ltd, SD4580, SD4584, SD4585, SD4560, SD4564, SD4565, SD4570, SD4574, SD4575, SD4600PFC, SD4593 and DC7651 ESIVE (trade names) available from Toyodo Corning Co., Ltd can be used together with the platinum (Pt) -based catalyst and the crosslinking agent described later.
(crosslinking agent)
The crosslinking agent is used for crosslinking an alkenyl group contained in the addition reaction type silicone adhesive. As the crosslinking agent, an organopolysiloxane (organohydrogenpolysiloxane) having at least 2, preferably 3 or more, hydrogen atoms (SiH) to which silicon atoms are bonded in 1 molecule is used.
Examples of the molecular structure of the organohydrogenpolysiloxane used as the crosslinking agent include linear, partially branched linear, branched chain, and network. The viscosity of the organohydrogenpolysiloxane at 25 ℃ is preferably in the range of 1 to 5,000 mPas.
The viscosity can be measured using a BM type rotational viscometer.
As the organohydrogenpolysiloxane used as the crosslinking agent, conventionally known ones can be used. For example, the organohydrogenpolysiloxane may be represented by the following general formula (3) or general formula (4), but is not limited thereto.
[ solution 3]
HbR3 (3-b)SiO-(HR3SiO)p-(R3 2SiO)q-SiR3 (3-b)HbGeneral formula (3)
[ solution 4]
Here, in the general formulae (3) and (4), R3Is a monovalent hydrocarbon group having 1 to 10 carbon atoms, b is 0 or 1, p and q are integers, and the viscosity of the organohydrogenpolysiloxane at 25 ℃ is 1 to 5,000 mPas. r is an integer of 2 or more, s is an integer of 0 or more, and r + s ≧ 3, preferably 8 ≧ r + s ≧ 3. The organohydrogenpolysiloxane may be a mixture of two or more kinds.
R3Is a monovalent hydrocarbon group having 1 to 10 carbon atoms, preferably 1 to 7 carbon atoms. Examples thereof include alkyl groups such as methyl, ethyl, propyl, and butyl; cycloalkyl groups such as cyclohexyl; and aryl groups such as phenyl and tolyl; vinyl and allyl. Particularly preferred is methyl or phenyl.
The content of the organohydrogenpolysiloxane used as a crosslinking agent in the adhesive layer 3 of the first embodiment is preferably an amount such that the total amount of silicon atom-bonded hydrogen atoms (SiH) in the organohydrogenpolysiloxane is in a range of 0.15mol equivalent to 15.0mol equivalent, and more preferably in a range of 1.0mol equivalent to 10.0mol equivalent, relative to the total amount of alkenyl groups in an organosilicon compound (G1) composed of an organopolysiloxane such as polydimethylsiloxane containing a silicon atom-bonded alkenyl group.
When the content of the organohydrogenpolysiloxane is less than the lower limit, the adhesive is less likely to be cured and the cohesive force is less likely to be increased when the adhesive tape 1 is irradiated with light. In this case, a desired lowering of the adhesive force and a failure mode in the holding force test cannot be obtained, and when the adhesive tape 1 is used for dicing of a semiconductor element substrate or the like and the obtained semiconductor chip or the like is peeled from the adhesive tape 1, there is a risk that the pickup property of the singulated semiconductor chip is deteriorated and the semiconductor chip or the like is likely to have adhesive residue.
On the other hand, when the content of the organohydrogenpolysiloxane exceeds the above upper limit value, there is a risk that the semiconductor chip is contaminated with the unreacted organohydrogenpolysiloxane. In addition, hydrogen atoms (SiH) bonded to silicon atoms in the unreacted organohydrogenpolysiloxane react with oxygen and moisture in the air to change to SiOH, and the adhesive force of the adhesive agent layer 3 to the adherend increases, which may deteriorate the pickup property of the singulated semiconductor chip.
As described above, the content of the crosslinking agent in the adhesive agent layer 3 according to the first embodiment may be adjusted so that the total amount of silicon atom-bonded hydrogen atoms (SiH) in the organohydrogenpolysiloxane is within the above range relative to the total amount of alkenyl groups in the silicone base (G1) composed of an organopolysiloxane such as polydimethylsiloxane containing silicon atom-bonded alkenyl groups.
The content of the crosslinking agent satisfying this range differs depending on the number of silicon atom-bonded hydrogen atoms (SiH) contained in the crosslinking agent, and for example, the crosslinking agent may be added so as to be in a range of 0.2 parts by mass or more and 20.0 parts by mass or less in terms of solid content with respect to 100 parts by mass of the solid content of the addition reaction type silicone-based adhesive.
When the content of the crosslinking agent is set to the above range with respect to the addition reaction type silicone adhesive, when the semiconductor chip is peeled off from the dicing adhesive tape, the photosensitive platinum (Pt) catalyst in the silicone adhesive can be activated by irradiating the adhesive layer 3 with light such as ultraviolet light, and the crosslinking reaction between the addition reaction type silicone adhesive and the crosslinking agent for the addition reaction type silicone adhesive is promoted, so that the cohesive force of the adhesive becomes larger than that before the light irradiation. As a result, the adhesive force of the adhesive layer 3 is appropriately reduced, good pickup properties can be achieved when peeling the semiconductor chip or the like from the adhesive tape 1, and adhesive residue on the semiconductor chip or the like can be suppressed.
The crosslinking agent is not particularly limited as long as it is used as a crosslinking agent for an addition reaction type silicone adhesive, that is, an organopolysiloxane (organohydrogenpolysiloxane) having at least 2 hydrogen atoms (SiH) to which silicon atoms are bonded in 1 molecule. Specific examples thereof include X-92-122 (trade name) manufactured BY shin-Etsu chemical Co., Ltd and BY24-741 (trade name) manufactured BY Toyo Corning Co., Ltd.
(photoactive platinum (Pt) catalysts)
The photosensitive platinum (Pt) catalyst is used for accelerating curing by an addition reaction (hydrosilylation) between an addition reaction type silicone adhesive constituting the adhesive agent layer 3 and a crosslinking agent by irradiation with light such as ultraviolet light. The wavelength of light that can be used to accelerate curing by the addition reaction of the addition-reaction-type silicone-based adhesive and the crosslinking agent is preferably in the range of 240nm to 400 nm.
As the photosensitive platinum (Pt) catalyst, a photoactive cyclopentadienyl platinum (IV) compound is preferably used in view of good photosensitivity and reaction rate.
The photoactive cyclopentadienylplatinum (IV) compound is not particularly limited, and examples thereof include (cyclopentadienyl) dimethyltrimethylsilylmethylplatinum, (cyclopentadienyl) diethyltrimethylsilylmethylplatinum, (cyclopentadienyl) dipropyltrimethylsilylmethylplatinum, (cyclopentadienyl) diisopropyltrimethylsilylplatinum, (cyclopentadienyl) diallyltrimethylsilylmethylplatinum, (cyclopentadienyl) dibenzyltrimethylsilylmethylplatinum, (cyclopentadienyl) dimethyltriethylsilylmethylplatinum, (cyclopentadienyl) dimethyltripropylsilylmethylplatinum, (cyclopentadienyl) dimethyltriisopropylsilylmethylplatinum, (cyclopentadienyl) dimethyltriphenylsilylmethylplatinum, (cyclopentadienyl) dimethylphenylsilylmethylplatinum, and the like, (cyclopentadienyl) dimethylmethyldiphenylsilylmethylplatinum, (cyclopentadienyl) dimethyldimethyl (trimethylsiloxy) silylmethylplatinum, (cyclopentadienyl) dimethyldimethyl (dimethylvinylsiloxy) silylmethylplatinum, [ (1 '-naphthyl) cyclopentadienyl ] trimethylsilylmethylplatinum, [ (2' -naphthyl) cyclopentadienyl ] trimethylsilylmethylplatinum, [ 1-methyl-3- (1 '-naphthyl) cyclopentadienyl ] trimethylsilylmethylplatinum, [ 1-methyl-3- (2' -naphthyl) cyclopentadienyl ] trimethylsilylmethylplatinum, [ (4 '-biphenyl) cyclopentadienyl ] trimethylsilylmethylplatinum, [1- (4' -biphenyl) -3-methylcyclopentadienyl ] trimethylsilylmethylplatinum Platinum, [ (9 '-phenanthryl) cyclopentadienyl ] trimethylsilylmethyl platinum, [ 1-methyl-3- (9' -phenanthryl) cyclopentadienyl ] trimethylsilylmethyl platinum, [1- (2 '-anthryl) -3-methylcyclopentadienyl ] trimethylsilylmethyl platinum, [ (2' -anthryl) cyclopentadienyl ] trimethylsilylmethyl platinum, [ (1 '-pyrenyl) cyclopentadienyl ] trimethylsilylmethyl platinum, [ 1-methyl-3- (1' -pyrenyl) cyclopentadienyl ] trimethylsilylmethyl platinum, and the like.
The cyclopentadienyl ring in the above compounds may be substituted with methyl, chloro, fluoro, trimethylsilyl, triethylsilyl, dimethylphenylsilyl, methyldiphenylsilyl, triphenylsilyl, phenyl, fluorophenyl, chlorophenyl, methoxy, naphthyl, biphenyl, anthryl, pyrenyl, 2-benzoylnaphthalene, thioxanthone, 2-chlorothioxanthone, 2-isopropylthioxanthone, anthraquinone, 1-chloroanthraquinone, acetophenone, benzophenone, 9, 10-dimethylanthracene, 9, 10-dichloroanthracene and a cyclopentadienyl ring substituted with 1 or more groups selected from these groups.
In the above compounds, the cyclopentadienyl ring may be substituted with η 5-fluorenyl.
The cyclopentadienyl ring in the above compound is preferably an unsubstituted cyclopentadienyl ring, a cyclopentadienyl ring substituted with one or more aromatic organic groups, a cyclopentadienyl ring substituted with one or more aliphatic organic groups, or a cyclopentadienyl ring substituted with one or more aromatic organic groups and one or more aliphatic organic groups. In addition, as the organic group which may be substituted with a cyclopentadienyl ring, naphthyl, biphenyl, anthryl, phenanthryl and pyrenyl are preferable.
The content of the photosensitive platinum (Pt) catalyst in the adhesive layer 3 of the first embodiment is not particularly limited as long as the addition reaction of the addition reaction type silicone adhesive and the crosslinking agent can be promoted by irradiation with light such as ultraviolet light. The content of the photosensitive platinum (Pt) catalyst in the adhesive layer 3 of the first embodiment is preferably in a range of 0.1 parts by mass or more and 3.0 parts by mass or less in terms of solid content, for example, relative to 100 parts by mass of the solid content of the addition reaction type silicone adhesive.
(cohesion builder)
The cohesive force-improving agent is used as needed to improve the cohesive force of the adhesive layer 3. The cohesive force enhancer is not particularly limited, and for example, a polyfunctional thiol is used. Examples of the cohesion improvement agent comprising a polyfunctional thiol include KARENZ (registered trademark) MT-PE1 and KARENZ MT-NR1 manufactured by Showa Denko K.K.K.
However, since the addition reaction type silicone adhesive is not compatible with the polyfunctional thiol, a compatibilizing agent for the addition reaction type silicone adhesive and the polyfunctional thiol is required in order to use the polyfunctional thiol as the cohesive force improver. The compatibilizing agent is not particularly limited, and examples thereof include KBM-802 and KBM-803 (both trade names) manufactured by shin-Etsu chemical Co., Ltd., and SH6062 (trade name) manufactured by Toureto Corning Ltd., as a silane coupling agent having a mercapto group.
When the cohesive force improver is used in the adhesive layer 3, the amount of the cohesive force improver added is preferably 6 parts by mass or less in terms of solid content, relative to 100 parts by mass of the solid content of the addition reaction type silicone adhesive. When the addition amount of the cohesion improvement agent exceeds 6 parts by mass in terms of solid content with respect to 100 parts by mass of the solid content of the addition reaction type silicone-based adhesive, the addition reaction type silicone-based adhesive may phase separate from the polyfunctional thiol as the cohesion improvement agent even if the compatibilizing agent is added.
(reinforcing Filler)
The reinforcing filler is used as needed to increase the strength of the adhesive layer 3. The reinforcing filler is not particularly limited, and examples thereof include AEROSIL (registered trademark) 130, AEROSIL 200, and AEROSIL 300, manufactured by AEROSIL corporation of Japan, REOLOSIL (registered trademark) QS-102, and REOLOSIL QS-30, manufactured by DSL, Inc. of Delshan, CARPLEX (registered trademark) 80, manufactured by DSL, and Hi-Sil (registered trademark) -233-D, manufactured by PPG.
< adhesive layer of the second embodiment >
The adhesive layer 3 of the second embodiment contains a peroxide-curable silicone adhesive in addition to the addition-reaction silicone adhesive, the crosslinking agent, and the photosensitive platinum (Pt) catalyst contained in the adhesive layer 3 of the first embodiment. The adhesive layer 3 of the second embodiment may further contain an initiator for initiating the polymerization reaction of the peroxide-curable silicone adhesive. Further, the adhesive agent layer 3 of the second embodiment may contain other additives such as a reinforcing filler, an cohesive force improving agent, and a colorant as necessary, similarly to the adhesive agent layer 3 of the first embodiment.
(peroxide-curable Silicone adhesive)
The peroxide-curable silicone adhesive can be any conventionally known adhesive, and is generally an adhesive containing a silicone gum (G2) composed of an organopolysiloxane such as polydimethylsiloxane and a silicone resin (R2) composed of an organopolysiloxane such as polydimethylsiloxane. Unlike the silicone gum (G2) contained in the addition reaction type silicone adhesive, the silicone gum (G1) composed of an organopolysiloxane contained in the peroxide curing type silicone adhesive does not generally contain an alkenyl group to which a silicon atom is bonded.
Hereinafter, the silicone gum (G2) composed of an organopolysiloxane such as polydimethylsiloxane having no alkenyl group to which a silicon atom is bonded, and the silicone resin (R2) composed of an organopolysiloxane such as polydimethylsiloxane, which are contained in the peroxide-curable silicone adhesive, will be described in further detail.
In the following description, a silicone gum (G2) composed of an organopolysiloxane such as polydimethylsiloxane that does not contain an alkenyl group to which a silicon atom is bonded may be simply expressed as a silicone gum (G2) composed of an organopolysiloxane such as polydimethylsiloxane.
[ Silicone rubber (G2) comprising organopolysiloxane such as polydimethylsiloxane having no silicon atom-bonded alkenyl group ]
The silicone gum (G2) composed of an organopolysiloxane such as polydimethylsiloxane in the present embodiment is not particularly limited as long as it is used for a peroxide-curable silicone adhesive, that is, a silicone gum that does not contain an alkenyl group to which a silicon atom is bonded. Examples of the molecular structure of such an organopolysiloxane include a linear structure having a main chain portion composed of diorganosiloxane repeating units, a structure in which a part of the molecular structure includes branched chains, a branched structure, or a cyclic structure.
The silicone gum (G2) composed of an organopolysiloxane such as polydimethylsiloxane which does not contain an alkenyl group to which a silicon atom is bonded may be oily or gel-like, and is preferably gel-like.
In the case of an oil, the viscosity of the silicone gum (G2) composed of an organopolysiloxane is preferably 1,000mPa · s or more at 25 ℃. When the viscosity is less than 1,000mPa · s, the adhesive before and after light irradiation may not exhibit desired adhesive properties, and the adhesion between the adhesive layer 3 and the substrate 2 may be deteriorated.
In the case of a raw gum, the viscosity of a silicone gum (G2) composed of an organopolysiloxane when dissolved in toluene at a concentration of 30 mass% is preferably 100,000mPa · s or less at 25 ℃. If the viscosity exceeds 100,000 mPas, stirring may become difficult in preparing the adhesive composition.
The viscosity can be measured using a BM type rotational viscometer.
Examples of the silicone gum (G2) composed of an organopolysiloxane such as polydimethylsiloxane containing no alkenyl group to which a silicon atom is bonded include those represented by the following general formula (5) or general formula (6), but are not limited thereto.
[ solution 5]
R4 3SiO-(R4 2SiO)t-SiR4 3General formula (5)
[ solution 6]
R4 2(OH)SiO-(R4 2SiO)t-SiR4 2(OH) general formula (6)
Here, in the above general formulae (5) and (6), R4Independently of each other, a monovalent hydrocarbon group having no aliphatic unsaturated bond, t is an integer of 100 or more, and the viscosity of the diorganopolysiloxane at 25 ℃ is 1,000 mPas or more.
As R4The monovalent hydrocarbon group having no aliphatic unsaturated bond and having 1 to 10 carbon atoms, preferably 1 to 7 carbon atoms, is preferable. Examples thereof include alkyl groups such as methyl, ethyl, propyl, and butyl; cycloalkyl groups such as cyclohexyl; and aryl groups such as phenyl and tolyl, and particularly preferably methyl.
[ Silicone resin (R2) comprising organopolysiloxane such as polydimethylsiloxane ]
The silicone resin (R2) composed of an organopolysiloxane such as polydimethylsiloxane in the present embodiment may be the same silicone resin as the silicone resin (R1) composed of an organopolysiloxane such as polydimethylsiloxane used in the addition reaction type silicone adhesive. Namely, a silicone resin comprising an organopolysiloxane such as polydimethylsiloxane(R2) is a group having R2 3SiO0.5Units (M units) and SiO2The organopolysiloxane of units (Q units) is called a so-called MQ resin. The silicone resin (R1) composed of this organopolysiloxane such as polydimethylsiloxane has substantially no alkenyl group in the molecule, and conventionally known ones can be used. R2A monovalent hydrocarbon group having 1 to 10 carbon atoms, and R is1Monovalent hydrocarbon groups are exemplified. The organopolysiloxanes mentioned are preferably those based on R2 3SiO0.5Unit/SiO2R is contained so that the molar ratio of the units is in the range of 0.5 to 1.72 3SiO0.5Unit and SiO2And (4) units. R2 3SiO0.5Unit/SiO2When the molar ratio of the unit is less than 0.5, the adhesive force or tackiness of the obtained adhesive agent layer 3 may decrease. On the other hand, if R2 3SiO0.5Unit/SiO2When the molar ratio of the unit exceeds 1.7, the adhesive force and holding power of the obtained adhesive agent layer 3 may decrease. The organopolysiloxane may have an OH group. In this case, the content of OH groups is preferably 4.0 mass% or less with respect to the total mass of the organopolysiloxane. If the OH group exceeds the above upper limit, the curability of the adhesive may be lowered.
In the present embodiment, in order to set the adhesive force of the adhesive tape 1 to 2.4N/10mm or more and 5.5N/10mm or less, MQ resin is preferably used as the silicone resin (R2) made of organopolysiloxane such as polydimethylsiloxane. However, the silicone resin (R2) composed of an organopolysiloxane such as polydimethylsiloxane may contain R as an impurity in the synthesis of MQ resin2SiO1.5Unit (T unit) and/or R2SiO unit (D unit).
The silicone gum (G2) composed of an organopolysiloxane such as polydimethylsiloxane having no alkenyl group to which a silicon atom is bonded and the silicone resin (R2) composed of an organopolysiloxane such as polydimethylsiloxane can also be used by simply mixing them. In addition, as the silicone compound (G2) composed of an organopolysiloxane such as polydimethylsiloxane not containing alkenyl groups to which silicon atoms are bonded, in the case where the organopolysiloxane represented by the above general formula (6) is contained, a silicone compound (G2) composed of an organopolysiloxane such as polydimethylsiloxane not containing alkenyl groups to which silicon atoms are bonded and a silicone resin (R2) composed of an organopolysiloxane such as polydimethylsiloxane may be used in the form of a (partial) condensation reaction product obtained by reacting in advance, as long as the characteristics of the present invention are not impaired.
(the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) contained in the adhesive layer of the second embodiment to the total mass (Rw) of the silicone resin (R), and the content ratio of the silicone gum (G1) having an alkenyl group to the total mass of the silicone gum (G) and the silicone resin (R))
As described above, the silicone adhesive constituting the adhesive layer 3 of the second embodiment includes an addition reaction type silicone adhesive and a peroxide curing type silicone adhesive. Therefore, in the silicone adhesive constituting the adhesive layer 3 of the second embodiment, the total mass (Gw) of the silicone gum (G) is the total mass (G1w) of the silicone gum (G1) composed of an organopolysiloxane such as polydimethylsiloxane containing an alkenyl group to which a silicon atom is bonded in the addition reaction type silicone adhesive and the mass (G2w) of the silicone gum (G2) composed of an organopolysiloxane such as polydimethylsiloxane not containing an alkenyl group to which a silicon atom is bonded in the peroxide curing type silicone adhesive. In the silicone adhesive constituting the adhesive layer 3 of the second embodiment, the total mass (Rw) of the silicone resin (R) is the total mass (R1w) of the mass (R1) of the silicone resin (R1) composed of an organopolysiloxane such as polydimethylsiloxane in the addition reaction type silicone adhesive and the mass (R2w) of the silicone resin (R2) composed of an organopolysiloxane such as polydimethylsiloxane in the peroxide curing type silicone adhesive.
The mass ratio (Gw)/(Rw) ((G1 w + G2w)/(R1w + R2w)) of the total mass (Gw) of the silicone gum (G) contained in the adhesive agent layer 3 of the second embodiment to the total mass (Rw) of the silicone resin (R) is preferably in the range of 40/60 to 56/44.
In this case, the content ratio { (G1w)/((Gw) + (Rw)) } × 100 of the silicone gum (G1) having an alkenyl group in the total mass of the silicone gum (G) and the silicone resin (R) is preferably in the range of 14 mass% or more and 42 mass% or less.
If the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) to the total mass (Rw) of the silicone resin (R) contained in the adhesive agent layer 3 of the second embodiment is less than the lower limit of the above range, the adhesive force or tackiness of the adhesive agent layer 3 may decrease. In this case, when the adhesive tape 1 is used for dicing a semiconductor element substrate, a fluorescent substrate, or the like, which will be described later, semiconductor chips or the like as cut pieces may scatter.
On the other hand, if the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) to the total mass (Rw) of the silicone resin (R) contained in the adhesive layer 3 of the second embodiment exceeds the upper limit of the above range, in the case where the mass of the silicone gum (G1) in the addition reaction type silicone-based adhesive is particularly large, the adhesive layer 3 becomes too soft due to the silicone gum (G) component in a state in which the adhesive before irradiation with light is uncured. In this case, when the semiconductor element substrate or the like is diced, the dicing vibration is easily transmitted to the adhesive layer 3, and the amplitude is increased, and there is a risk that the semiconductor element substrate is displaced from the reference position, for example. Further, there is a risk that fragments (chips) are generated on the singulated semiconductor chips, and there is a risk that size variations occur in each individual semiconductor chip.
In addition, when the silicone rubber (G2) in the peroxide-curable silicone adhesive is particularly high in mass, curing of the peroxide-curable silicone adhesive by an initiator is likely to proceed, and the adhesive force or tackiness of the adhesive layer 3 may decrease. In this case, when the adhesive tape 1 is used for dicing a semiconductor element substrate, a fluorescent substrate, or the like, which will be described later, semiconductor chips or the like as cut pieces may scatter.
If the content ratio of the silicone gum (G1) having an alkenyl group in the adhesive layer 3 of the second embodiment in the total mass of the silicone gum (G) and the silicone resin (R) is less than the lower limit of the above range, the adhesive is less likely to be cured and the cohesive force is less likely to be increased when the adhesive tape 1 is irradiated with light. In this case, a desired lowering of the adhesive force and a failure mode in the holding force test cannot be obtained, and there is a risk that the pickup property of the singulated semiconductor chip is deteriorated and the semiconductor chip and the like are likely to generate adhesive residue when the obtained semiconductor chip and the like are peeled from the adhesive tape 1 after the adhesive tape 1 is used for dicing of the semiconductor element substrate and the like.
On the other hand, if the content ratio of the silicone gum (G1) having an alkenyl group in the adhesive layer 3 of the second embodiment in the total mass of the silicone gum (G) and the silicone resin (R) exceeds the upper limit value of the above range, the adhesive layer 3 becomes too soft due to the silicone gum (G) component in a state in which the adhesive before irradiation with light is uncured. In this case, when the semiconductor element substrate or the like is diced, the dicing vibration is easily transmitted to the adhesive layer 3, and the amplitude is increased, so that there is a risk that the semiconductor element substrate is displaced from the reference position, for example. In addition, there is a risk that fragments (fragments) are generated on the singulated semiconductor chips, and there is a risk that size variations occur on the individual semiconductor chips.
The content of the peroxide-curable silicone adhesive in the adhesive layer 3 of the second embodiment may be adjusted by considering the ratio of the silicone gum (G2) and the silicone resin (R2) of the peroxide-curable silicone adhesive so that the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) and the total mass (Rw) of the silicone resin (R) contained in the adhesive layer of the second embodiment and the content ratio of the silicone gum (G1) having an alkenyl group in the total mass of the silicone gum (G) and the silicone resin (R) are within the above range when mixed with the addition reaction type silicone adhesive.
By setting the content of the peroxide silicone adhesive in the adhesive layer 3 of the second embodiment to the above range, when the adhesive tape 1 is used for dicing a semiconductor element substrate, a fluorescent substrate, or the like, scattering of semiconductor chips or the like as cut pieces can be suppressed, and adhesive residue can be suppressed when the adhesive tape 1 is peeled off.
Further, as the peroxide-curable silicone adhesive of the present invention, a commercially available peroxide-curable silicone adhesive may be used. Specific examples thereof include KR100 and KR101-10 (trade names), YR3340, YR3286, PSA610-SM, XR37-B6722 (trade names), both of which are available from shin-Etsu chemical Co., Ltd., and SH4280, SH4282, SE4200, BY24-717, BY24-715, and Q2-7735 (trade names), all of which are available from Toyo Corning Co., Ltd.).
(initiator)
As the initiator, a peroxide, more specifically, an organic peroxide can be used. Examples of the organic peroxide used as the initiator include, but are not particularly limited to, benzoyl peroxide, dicumyl peroxide, 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane, 1' -di-t-butylperoxy-3, 3, 5-trimethylenecyclohexane, and 1, 3-di- (t-butylperoxy) -diisopropylbenzene, and examples of commercially available products include NYPER K40 manufactured by Nikkiso K.K.K.K.K.K.K.K.K.K.K.K.K.K.K.K.K.K.K.K.K.K.
The content of the initiator in the adhesive layer 3 of the second embodiment is preferably 10 parts by mass or less in terms of solid content per 100 parts by mass of the solid content of the peroxide-curable silicone adhesive. When the content of the initiator in the adhesive layer 3 of the second embodiment exceeds 10 parts by mass in terms of solid content relative to 100 parts by mass of the solid content of the peroxide-curable silicone adhesive, the curing reaction of the peroxide-curable silicone adhesive in the adhesive layer 3 may excessively proceed. In this case, the adhesive layer 3 becomes hard, and the adhesive force of the adhesive tape 1 is likely to decrease. When the adhesive tape 1 is used for dicing a semiconductor element substrate or the like, semiconductor chips or the like as cut pieces may be easily peeled off from the adhesive tape 1 and scattered when the semiconductor element substrate or the like is cut.
< thickness >
The thickness of the adhesive layer 3 is preferably in the range of 10 μm to 100 μm, and more preferably in the range of 20 μm to 40 μm. When the thickness of the adhesive layer 3 is less than 10 μm, the thickness of the silicone adhesive contained in the adhesive layer 3 becomes small, and thus the adhesive force of the adhesive tape 1 is likely to decrease. On the other hand, when the thickness of the adhesive layer 3 is larger than 100 μm, the adhesive layer 3 may be easily broken by aggregation. Further, when the adhesive tape 1 is used for dicing a semiconductor element substrate or the like and then the obtained semiconductor chip or the like is peeled off from the adhesive tape 1, there is a risk that adhesive residue is likely to occur in the semiconductor chip or the like. In addition, when dicing a semiconductor element substrate or the like, the dicing vibration is easily transmitted to the adhesive layer 3, and the amplitude is increased, which may cause the semiconductor element substrate to be displaced from a reference position, for example. In addition, there is a risk that fragments (fragments) are generated on the singulated semiconductor chips, and there is a risk that size variations occur on the individual semiconductor chips.
< adhesion promoting coating >
As described above, in the adhesive tape 1 of the present embodiment, a tack coat layer corresponding to the type of the substrate 2 may be provided between the substrate 2 and the adhesive layer 3 or a surface treatment such as a corona treatment may be performed depending on the production conditions of the adhesive tape 1, the use conditions of the adhesive tape 1 after production, and the like. This improves the adhesion between the substrate 2 and the adhesive layer 3.
< surface treatment >
The surface of the substrate 2 (the surface opposite to the surface facing the adhesive layer 3) may be subjected to a surface treatment such as a release property improving treatment. The treating agent used for the surface treatment of the substrate 2 is not particularly limited, and for example, a non-silicone release treating agent such as a long-chain alkyl vinyl monomer polymer, a fluoroalkyl vinyl monomer polymer, polyvinyl alcohol urethane, and a urethane resin can be used. Examples of such a non-silicone-based release treatment agent include PEELOIL 1050 and PEELOIL 1200 manufactured by oil and fat industries co.
< Release liner >
Further, a release liner may be provided as necessary on the surface of the adhesive layer 3 (the surface opposite to the surface facing the substrate 2). As the release liner, the following release liners can be used: a release liner subjected to a release treatment for improving releasability from a silicone adhesive contained in the adhesive layer 3 is applied to a film such as paper, polyethylene, polypropylene, or polyethylene terephthalate. The material used for the release treatment of the release liner is not particularly limited, and examples thereof include fluoroalkyl-modified silicones, long-chain alkyl vinyl monomer polymers, and amino alkyd resins.
Thickness of adhesive tape
The thickness of the entire adhesive tape 1 having the above-described structure is preferably in a range of 20 μm to 200 μm.
When the thickness of the adhesive tape 1 is less than 20 μm, it may be difficult to peel off the formed semiconductor chip or the like from the adhesive tape 1 when the adhesive tape 1 is used for dicing a semiconductor element substrate or the like.
On the other hand, when the thickness of the adhesive tape 1 exceeds 200 μm, the adhesive tape 1 is difficult to follow the irregularities formed on the bonding surface of the semiconductor element substrate when the adhesive tape 1 is bonded to the semiconductor element substrate or the like. In this case, the adhesive tape 1 has a small bonding area with the semiconductor element substrate and the like, and the semiconductor chip and the like may easily scatter during dicing.
[ method for producing adhesive tape ]
Next, a method for producing the adhesive tape 1 of the present embodiment will be described. The method for producing the adhesive tape 1 described below is an example, and the method for producing the adhesive tape 1 is not limited to this.
Here, the adhesive tape 1 of the first embodiment in which the adhesive layer 3 contains an addition reaction type silicone adhesive as a curable silicone adhesive and the adhesive tape 1 of the second embodiment in which the adhesive layer 3 contains an addition reaction type silicone adhesive and a peroxide curable silicone adhesive as curable silicone adhesives can be manufactured by the same manufacturing method.
In manufacturing the adhesive tape 1, first, other components such as a curable silicone adhesive and a crosslinking agent are dissolved in a common organic solvent such as toluene and ethyl acetate to obtain an adhesive solution. Next, the adhesive solution is applied to the surface of the substrate 2, which is surface-treated and given a tack coat as necessary, so as to have a predetermined thickness by using a notch wheel coater or the like.
Next, the substrate 2 coated with the adhesive solution is heated at a temperature of 60 to 160 ℃ for several to several tens of minutes to dry and cure the adhesive solution, thereby forming the adhesive layer 3.
Through the above steps, an adhesive tape 1 in which an adhesive layer 3 is laminated on a substrate 2 as shown in fig. 1 is obtained.
[ method of Using adhesive tape ]
The adhesive tape 1 of the present embodiment is used for dicing a semiconductor material as a semiconductor chip material in a manufacturing process of a semiconductor chip having a semiconductor element such as an led (light emitting diode) or a power semiconductor.
Specifically, the adhesive tape 1 is used for dicing a semiconductor element substrate in which a plurality of semiconductor elements such as LED elements and power semiconductor elements are formed on a substrate made of resin, ceramic, or the like, to obtain singulated semiconductor chips. Here, in a semiconductor element substrate having a plurality of semiconductor elements formed on a substrate, a sealing resin, which is an example of a coating material, may be provided so as to cover the semiconductor elements in order to protect the semiconductor elements from external environments such as temperature and humidity.
The adhesive tape 1 of the present embodiment can be more preferably used for dicing a semiconductor element substrate provided with a sealing resin.
As a method for obtaining a plurality of semiconductor chips by cutting a semiconductor element substrate provided with a sealing resin, for example, the following method is known.
First, an adhesive tape for dicing is attached from the substrate side of the semiconductor element substrate, and the semiconductor element substrate is cut from the side where the semiconductor element is formed by a dicing machine or the like. Then, each of the semiconductor chips formed by cutting is peeled off from the adhesive tape, thereby obtaining a plurality of semiconductor chips.
However, when the dicing adhesive tape is attached from the substrate side of the semiconductor element substrate and the semiconductor element substrate is cut, there are problems such as occurrence of so-called sagging (ダレ) which causes detachment at the cut surface (substrate side surface of the semiconductor chip), and roughening of the cut surface.
In order to solve such problems, the following methods have been proposed in recent years: for the semiconductor element substrate, an adhesive tape for dicing is attached from the side where the semiconductor element is formed, that is, the side of the sealing resin sealing the semiconductor element, instead of from the substrate side, and the semiconductor element substrate is cut.
Here, as a sealing resin for a semiconductor element such as an LED or a power semiconductor, an epoxy resin having excellent electrical characteristics and heat resistance has been conventionally used, but the epoxy resin has the following problems: when used for high-output LEDs and power semiconductors, when used for short-wavelength LEDs, or due to the use environment of semiconductor chips, discoloration is likely to occur.
In recent years, silicone resins have been used in many cases as sealing resins for semiconductor elements such as LEDs and power semiconductors because they are less likely to be discolored by heat or light than epoxy resins. More specifically, silicone resins containing both or one of a methyl group and a phenyl group as a functional group, that is, silicone resins containing a methyl group, silicone resins containing a phenyl group, and silicone resins containing both a methyl group and a phenyl group are often used.
By using a silicone resin as a sealing resin for a semiconductor element, discoloration of the sealing resin due to heat or light can be suppressed.
In addition, the light transmittance of the organic silicon resin is more than 88% (wavelength is 400-800 nm), and the refractive index is more than 1.41. Therefore, when the semiconductor element is an LED, the light emitted from the LED can be efficiently extracted to the outside of the package by using the silicone resin as the sealing resin. Among the above-mentioned silicone resins, the use of a silicone resin containing a phenyl group can achieve further efficiency of emitted light than the use of a silicone resin containing a methyl group.
The methyl group-containing silicone resin is not particularly limited, and examples thereof include KER-2300, KER-2460, KER-2500N, KER-2600, KER-2700, KER-2900, X-32-2528, IVS4312, XE14-C2042, IVS4542, IVS4546, IVS4622, IVS4632, IVS4742, IVS4752, IVSG3445, IVSG0810, IVSG5778, XE13-C2479, IVSM4500, OE-6351, OE-6336, and OE-6301 available from Toho chemical industries, Ltd.
The silicone resin containing a methyl group and a phenyl group is not particularly limited, and examples thereof include KER-6075, KER-6150 and KER-6020 manufactured by shin-Etsu chemical Co., Ltd.
The phenyl group-containing silicone resin is not particularly limited, and examples thereof include KER-6110, KER-6000, KER-6200, ASP-1111, ASP-1060, ASP-1120, ASP-1050P, XE14-C2508 manufactured by shin-Etsu chemical Co., Ltd., OE-6520, OE-6550, OE-6631, OE-6636, OE-6635, OE-6630 and the like manufactured by Toyo Corning Co., Ltd.
In addition, conventionally, as an adhesive tape for dicing for cutting a semiconductor element, for example, an adhesive tape in which an adhesive layer is made of an acrylic resin-based adhesive has been used.
However, if such a conventional adhesive tape is attached from the side of the semiconductor element substrate on which the semiconductor element is formed (the side of the sealing resin) and the semiconductor element substrate is diced, for example, if the adhesive force between the sealing resin and the adhesive tape is insufficient, there is a possibility that the semiconductor chip is scattered during dicing.
In particular, the silicone resin has a property of having a high mold releasability as compared with, for example, an epoxy resin or the like which has been conventionally used as a sealing resin. Therefore, when an adhesive tape in which an adhesive layer is made of an acrylic resin-based adhesive is attached to a semiconductor element substrate using a silicone resin as a sealing resin, for example, the adhesion between the silicone resin as the sealing resin and the adhesive tape tends to be small. As a result, problems such as scattering of semiconductor chips are more likely to occur when the semiconductor element substrate is diced.
In contrast, in the adhesive tape 1 of the present embodiment, since the adhesive layer 3 is configured to include the silicone-based adhesive in which the silicone base (G) and the silicone resin (R) are mixed at an appropriate ratio as described above, it is possible to maintain the adhesive force and the adhesive force with the sealing resin of the semiconductor element substrate in a good state even when the semiconductor element substrate is used by being stuck from the sealing resin side made of the silicone resin when the semiconductor element substrate is cut. Further, compared to conventional adhesive tapes, the semiconductor element substrate can be cut while suppressing the occurrence of scattering of semiconductor chips.
On the other hand, the adhesive layer 3 contains the silicone adhesive, the photosensitive platinum (Pt) catalyst and the crosslinking agent, and thus, by irradiation with light such as ultraviolet light, the photosensitive platinum (Pt) catalyst in the silicone adhesive is activated, and the crosslinking reaction between the addition reaction type silicone adhesive and the crosslinking agent for the addition reaction type silicone adhesive is promoted, so that the cohesive force of the adhesive becomes larger than before the light irradiation. As a result, the adhesive force of the adhesive layer 3 is appropriately reduced, and the failure mode in the retention test is "interfacial peeling" or "no drop" in the retention test. This makes it possible to achieve good pickup properties when peeling the semiconductor chip or the like from the adhesive tape 1, and also to suppress adhesive residue on the semiconductor chip or the like.
Hereinafter, a method of using the adhesive tape 1 of the present embodiment and a method of manufacturing a semiconductor chip using the adhesive tape 1 of the present embodiment will be described in detail. Fig. 2(a) to (e) are views showing a method for manufacturing a semiconductor chip using the adhesive tape 1 of the present embodiment.
Here, a case where a semiconductor chip having an LED element as a semiconductor element is manufactured using the adhesive tape 1 will be described as an example. The method described below is an example of a method of using the adhesive tape 1 and a method of manufacturing a semiconductor chip using the adhesive tape 1, but the method is not limited to the method described below.
In the present embodiment, first, a plurality of semiconductor elements 102 are mounted on a substrate 101 made of, for example, a resin material, ceramic, or the like, to produce a semiconductor element substrate 100. The semiconductor element 102 is, for example, an LED element, and although not shown, is configured by stacking a plurality of semiconductor layers including, for example, a light-emitting layer that emits light when energized, and an electrode is formed on the upper portion.
Next, the plurality of semiconductor elements formed on the substrate 101 of the semiconductor element substrate 100 are sealed with a sealing resin 103 made of a silicone resin (sealing step). In this example, the plurality of semiconductor elements 102 are collectively sealed with the sealing resin 103, but each semiconductor element 102 may be separately sealed with the sealing resin 103.
Next, as shown in fig. 2(a), the adhesive tape 1 and the semiconductor element substrate 100 are bonded so that the adhesive layer 3 of the adhesive tape 1 faces the sealing resin 103 of the semiconductor element substrate 100 (bonding step).
Next, as shown in fig. 2(b) and (c), the semiconductor element substrate 100 is cut along the lines to cut X by a dicing saw or the like in a state where the adhesive tape 1 is bonded to the semiconductor element substrate 100 (cutting step). In this example, the semiconductor element substrate 100 to which the adhesive tape 1 is attached is cut from the substrate 101 side. In this example, as shown in fig. 2(c), so-called full dicing is performed in which the semiconductor element substrate 100 is cut into all portions in the thickness direction.
Next, as shown in fig. 2 d, the pressure-sensitive adhesive tape 1 attached to the semiconductor element substrate 100 is irradiated with ultraviolet rays from the base material 2 side (ultraviolet irradiation step). As described above, the base material 2 is made of a material that transmits ultraviolet rays. Therefore, by irradiating the adhesive tape 1 with ultraviolet light from the substrate 2 side, the ultraviolet light is transmitted through the substrate 2 and irradiated to the adhesive layer 3.
In the adhesive tape 1 of the present embodiment, since the adhesive agent layer 3 has a photosensitive platinum (Pt) catalyst, the addition reaction of the addition reaction type silicone adhesive and the crosslinking agent in the adhesive agent layer 3 can be promoted by irradiating the adhesive agent layer 3 with ultraviolet rays. This increases the crosslinking density, i.e., cohesive force, in the adhesive layer 3 as compared to before the irradiation with ultraviolet rays, and reduces the adhesive force of the adhesive layer 3.
Next, the semiconductor chip 200 formed by cutting the semiconductor element substrate 100 is peeled (picked up) from the adhesive tape 1, and as shown in fig. 2(e), a singulated semiconductor chip 200 can be obtained (peeling step).
As described above, in the adhesive tape 1 of the present embodiment, the adhesive layer 3 is configured to include the silicone adhesive in which the silicone base (G) and the silicone resin (R) are mixed at an appropriate ratio. Thus, when the adhesive tape 1 is used for dicing, the adhesive force and adhesive force between the adhesive tape 1 and the semiconductor element substrate 100 can be favorably maintained.
In particular, in recent years, silicone resins having high releasability are often used as the sealing resin 103 for sealing the semiconductor element 102. In contrast, the adhesive tape 1 of the present embodiment has the above-described configuration, and thus has good adhesive force and adhesive force even to the sealing resin 103 made of silicone resin.
As a result, the adhesive tape 1 of the present embodiment can suppress scattering of the semiconductor chip 200 when used for dicing the semiconductor element substrate 100.
Further, the silicone adhesive contained in the adhesive layer 3 of the adhesive tape 1 of the present embodiment has good adhesion to the sealing resin 103 as described above, and has high releasability.
Further, the adhesive tape 1 of the present embodiment includes, for example, a photosensitive platinum (Pt) catalyst that promotes an addition reaction between an addition reaction type silicone adhesive and a crosslinking agent by irradiation with light such as ultraviolet light. Further, by irradiating the adhesive layer 3 with light through the base material 2 after the cutting step and before the peeling step, the addition reaction of the addition-reactive silicone adhesive and the crosslinking agent in the adhesive layer 3 can be promoted, the cohesive force can be increased, and the adhesive force of the adhesive layer 3 can be reduced. Thus, in the peeling step, when the semiconductor chip 200 obtained by dicing the semiconductor element substrate 100 is peeled (picked up) from the adhesive tape 1, the occurrence of so-called adhesive residue in which the adhesive adheres to the semiconductor chip 200 can be suppressed. In addition, good pickup properties when peeling the semiconductor chip 200 from the adhesive tape 1 can be achieved.
The method of obtaining the singulated semiconductor chips by attaching the adhesive tape 1 from the sealing resin side and cutting the semiconductor element substrate having the plurality of semiconductor elements formed on the substrate has been described above. However, the use of the adhesive tape 1 of the present embodiment is not limited thereto.
The adhesive tape 1 of the present embodiment may be used, for example, in the manufacture of a chip-scale packaged LED, for dicing a semiconductor material in which a plurality of LED elements are covered with a phosphor as an example of a coating material to obtain a singulated chip-scale packaged LED. The phosphor is a member in which a fluorescent material is dispersed in a resin material, ceramic, or the like.
In recent years, with the miniaturization of chip scale packaged LEDs, there is a tendency that the chip scale packaged LEDs that have been singulated during dicing are easily scattered. In contrast, by using the adhesive tape 1 of the present embodiment having the above-described configuration, the adhesion between the phosphor and the adhesive layer 3 can be maintained well, and scattering of the singulated chip-scale package LED can be suppressed.
Further, by irradiating the adhesive layer 3 with ultraviolet rays after dicing to reduce the adhesive force, the singulated chip scale package LED can be easily peeled from the adhesive tape 1, and the occurrence of adhesive residue on the peeled chip scale package LED can be suppressed.
Examples
Next, the present invention will be described in further detail with reference to examples and comparative examples. The present invention is not limited to the following examples.
The present inventors prepared an adhesive tape 1 by varying the composition, thickness of each layer, and the like of the adhesive layer 3, and evaluated the prepared adhesive tape 1, for each of a first embodiment in which the adhesive layer 3 contains an addition reaction type silicone adhesive as a curable silicone adhesive, and a second embodiment in which the adhesive layer 3 contains an addition reaction type silicone adhesive and a peroxide curable silicone adhesive as curable silicone adhesives. In the following examples, examples 1 to 8 correspond to the first aspect, and examples 9 to 15 correspond to the second aspect.
Hereinafter, each example and each comparative example will be described in detail.
1. Production of adhesive tape 1
(example 1)
Toluene, 166.67 parts BY mass of an addition reaction type silicone adhesive (a crosslinking agent not added, having a solid content concentration of 60% BY mass, manufactured BY Torredo Corning corporation SD4584 (trade name)) composed of an organopolysiloxane having a vinylsilyl group as a silicon atom-bonded alkenyl group in a molecule, and 3.30 parts BY mass of a crosslinking agent (BY 24-741 (trade name, manufactured BY Torredo Corning corporation, having a solid content concentration of 20% BY mass)) composed of an organopolysiloxane having a hydrosilyl group in a molecule were mixed and stirred. Subsequently, 5.33 parts by mass of a solution of a photosensitive platinum (Pt) catalyst (trimethyl (methylcyclopentadienyl) platinum (IV) manufactured by Sigma Aldrich japan contract corporation) diluted with toluene to a solid content concentration of 15% by mass was added, and mixed and stirred to prepare an adhesive solution of the first embodiment.
Subsequently, the adhesive solution was applied to a substrate 2 made of a polyethylene terephthalate (PET) film having a thickness of 38 μm, and then heated at a temperature of 120 ℃ for 3 minutes to form an adhesive layer 3 having a thickness of 20 μm after drying. Thus, an adhesive tape 1 having a total thickness of 58 μm after drying was obtained.
(example 2)
In the preparation of the adhesive solution of the first embodiment, an addition reaction type silicone adhesive (a crosslinking agent not added, SD4584 (trade name) manufactured by tokyo kening corporation, having a vinylsilyl group in the molecule, having a solid content concentration of 60 mass%) composed of an organopolysiloxane having a silicon atom-bonded alkenyl group was used, and the thickness of the adhesive layer 3 after drying was set to 30 μm, and an adhesive tape 1 having a total thickness of 68 μm after drying was obtained in the same manner as in example 1.
(example 3)
An adhesive tape 1 having a total thickness of 22 μm after drying was obtained in the same manner as in example 2, except that a PET film having a thickness of 12 μm was used as the substrate 2 and the thickness of the adhesive layer 3 after drying was set to 10 μm.
(example 4)
In preparation of the adhesive solution of the first embodiment, an addition reaction type silicone adhesive (a crosslinking agent not added, with a solid content concentration of 60 mass%) composed of an organopolysiloxane having a vinylsilyl group as an alkenyl group to which a silicon atom is bonded, which is a product of SD4585 (trade name) manufactured by tokyo ken corporation) in a molecule was used as the base 2, a PET film having a thickness of 50 μm was used, and the thickness of the adhesive layer 3 after drying was set to 40 μm, and an adhesive tape 1 having a total thickness of 90 μm after drying was obtained in the same manner as in example 1.
(example 5)
An adhesive tape 1 having a total thickness of 58 μm after drying was obtained in the same manner as in example 1 except that the amount of the crosslinking agent (BY 24-741 (trade name, solid content concentration: 20% BY mass), manufactured BY Torreken corporation, was changed to 1.65 parts BY mass in the preparation of the adhesive solution of the first embodiment.
(example 6)
An adhesive tape 1 having a total thickness of 58 μm after drying was obtained in the same manner as in example 1 except that the amount of the crosslinking agent (BY 24-741 (trade name, solid content concentration: 20% BY mass), manufactured BY Torreken corporation, was 8.25 parts BY mass in the preparation of the adhesive solution of the first embodiment.
(example 7)
An adhesive tape 1 having a total thickness of 58 μm after drying was obtained in the same manner as in example 1 except that the amount of the photosensitive platinum (Pt) catalyst (trimethyl (methylcyclopentadienyl) platinum (IV) manufactured by Sigma Aldrich japan contract corporation) diluted with toluene to a solid content concentration of 15 mass% was changed to 2.00 parts by mass in preparation of the adhesive solution of the first embodiment.
(example 8)
An adhesive tape 1 having a total thickness of 58 μm after drying was obtained in the same manner as in example 1 except that the amount of the solution of the photosensitive platinum (Pt) catalyst (trimethyl (methylcyclopentadienyl) platinum (IV) manufactured by Sigma Aldrich japan contract corporation) diluted with toluene to a solid content concentration of 15 mass% was 20.00 parts by mass.
(example 9)
Toluene, 166.67 parts BY mass of an addition reaction type silicone adhesive (a crosslinking agent not added, having a solid content concentration of 60% BY mass, manufactured BY Torredo Corning corporation SD4584 (trade name)) composed of an organopolysiloxane having a vinylsilyl group as a silicon atom-bonded alkenyl group in a molecule, and 3.30 parts BY mass of a crosslinking agent (BY 24-741 (trade name, manufactured BY Torredo Corning corporation, having a solid content concentration of 20% BY mass)) composed of an organopolysiloxane having a hydrosilyl group in a molecule were mixed and stirred. Subsequently, 5.33 parts by mass of a solution of a photosensitive platinum (Pt) catalyst (trimethyl (methylcyclopentadienyl) platinum (IV) manufactured by Sigma Aldrich japan contract corporation) diluted with toluene to a solid content concentration of 15% by mass was added, and mixed and stirred to prepare an addition reaction type silicone adhesive solution.
On the other hand, toluene, 166.67 parts by mass of a peroxide-curable silicone adhesive (SH 4280 (trade name) manufactured by toyodo corning co., ltd., solid content concentration 60 mass%), and 5.00 parts by mass of an initiator (NYPER K40 (trade name) manufactured by nippon oil co., ltd., solid content concentration 40 mass%) made of methyl benzoyl peroxide were mixed and stirred to prepare a peroxide-curable silicone adhesive solution.
Next, the obtained addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution were mixed and stirred to prepare an adhesive solution of the second embodiment. The mixing ratio of the addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution was adjusted so that 100 parts by mass (solid content) of the peroxide curing type silicone adhesive was contained per 100 parts by mass (solid content) of the addition reaction type silicone adhesive.
Subsequently, the adhesive solution was applied to a substrate 2 made of a polyethylene terephthalate (PET) film having a thickness of 38 μm, and then heated at 160 ℃ for 3 minutes to form an adhesive layer 3 having a thickness of 20 μm after drying. Thus, an adhesive tape 1 having a total thickness of 58 μm after drying was obtained.
(example 10)
In preparation of the adhesive solution according to the second embodiment, an adhesive tape 1 having a total thickness of 58 μm after drying was obtained in the same manner as in example 9 except that the mixing ratio of the addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution was adjusted so as to contain 63.70 parts by mass (solid content) of the peroxide curing type silicone adhesive per 100 parts by mass (solid content) of the addition reaction type silicone adhesive.
(example 11)
In preparation of the adhesive solution according to the second embodiment, an adhesive tape 1 having a total thickness of 58 μm after drying was obtained in the same manner as in example 9 except that the mixing ratio of the addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution was adjusted so as to contain 150 parts by mass (solid content) of the peroxide curing type silicone adhesive per 100 parts by mass (solid content) of the addition reaction type silicone adhesive.
(example 12)
In preparation of the addition reaction type silicone adhesive solution of the second embodiment, an adhesive tape 1 having a total thickness of 58 μm after drying was obtained in the same manner as in example 9 except that as the addition reaction type silicone adhesive composed of an organopolysiloxane having a vinylsilyl group as an alkenyl group to which a silicon atom is bonded in the molecule, an unadditized crosslinking agent type (solid content concentration 60 mass%) SD4580 (trade name) manufactured by tokyo kening co.
(example 13)
In preparation of the addition reaction type silicone adhesive solution of the second embodiment, an adhesive tape 1 having a total thickness of 58 μm after drying was obtained in the same manner as in example 9 except that as the addition reaction type silicone adhesive composed of an organopolysiloxane having a vinylsilyl group as an alkenyl group to which a silicon atom is bonded in the molecule, an unadditized crosslinking agent type (solid content concentration 60 mass%) SD4586 (trade name) manufactured by tokyo kening co.
(example 14)
Toluene, 166.67 parts BY mass of an addition reaction type silicone-based adhesive composed of an organopolysiloxane having a vinylsilyl group as an alkenyl group to which a silicon atom is bonded in the molecule (an unadditized crosslinking agent type of SD4585 (trade name) manufactured BY tokyo ken corporation, solid content concentration 60 mass%), and 3.30 parts BY mass of a crosslinking agent composed of an organopolysiloxane having a hydrosilyl group in the molecule (BY 24-741 (trade name) manufactured BY tokyo ken corporation, solid content concentration 20 mass%) were mixed and stirred. Subsequently, 5.33 parts by mass of a solution of a photosensitive platinum (Pt) catalyst (trimethyl (methylcyclopentadienyl) platinum (IV) manufactured by Sigma Aldrich japan contract corporation) diluted with toluene to a solid content concentration of 15% by mass was added, and mixed and stirred to prepare an addition reaction type silicone adhesive solution.
On the other hand, toluene and 166.67 parts BY mass of a peroxide-curable silicone adhesive (BY 24-717 (trade name), solid content concentration: 60% BY mass, manufactured BY Torreken corporation) were mixed and stirred to prepare a peroxide-curable silicone adhesive solution.
Next, the obtained addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution were mixed and stirred to prepare an adhesive solution of the second embodiment. The mixing ratio of the addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution was adjusted so that 20 parts by mass (solid content) of the peroxide curing type silicone adhesive was contained per 100 parts by mass (solid content) of the addition reaction type silicone adhesive.
Subsequently, the adhesive solution was applied to a substrate 2 made of a polyethylene terephthalate (PET) film having a thickness of 38 μm, and then heated at 160 ℃ for 3 minutes to form an adhesive layer 3 having a thickness of 20 μm after drying. Thus, an adhesive tape 1 having a total thickness of 58 μm after drying was obtained.
(example 15)
First, an addition reaction type silicone adhesive solution was prepared in the same manner as the adhesive solution of the first embodiment of example 4.
On the other hand, toluene, 250.00 parts by mass of a peroxide-curable silicone adhesive (SE 4200 (trade name) made by tokyo ken corporation, solid content concentration 40 mass%) composed of an organopolysiloxane, and 5.00 parts by mass of an initiator (NYPER K40 (trade name) made by nikkaido corporation, solid content concentration 40 mass%) composed of methyl benzoyl peroxide were mixed and stirred to prepare a peroxide-curable silicone adhesive solution.
Next, the obtained addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution were mixed and stirred to prepare an adhesive solution of the second embodiment. The mixing ratio of the addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution was adjusted so that 150 parts by mass (solid content) of the peroxide curing type silicone adhesive was contained per 100 parts by mass (solid content) of the addition reaction type silicone adhesive.
Subsequently, the adhesive solution was applied to a substrate 2 made of a polyethylene terephthalate (PET) film having a thickness of 125 μm, and then heated at 160 ℃ for 3 minutes to form an adhesive layer 3 having a thickness of 20 μm after drying. Thus, an adhesive tape 1 having a total thickness of 145 μm after drying was obtained.
Comparative example 1
An adhesive tape 1 having a total thickness of 73 μm after drying was obtained in the same manner as in example 1, except that 6 parts by mass of a platinum metal catalyst (NC-25 (trade name), 25% by mass in solid content, manufactured by toray corning) was used instead of the solution of the photosensitive platinum (Pt) catalyst (trimethyl (methylcyclopentadienyl) platinum (IV), manufactured by Sigma Aldrich japan contract corporation), and the thickness of the adhesive layer 3 after drying was 35 μm.
Comparative example 2
An adhesive tape 1 having a total thickness of 68 μm after drying was obtained in the same manner as in example 1 except that 10.00 parts by mass of YF3897 (trade name), which is a linear polyorganosiloxane having silanol groups at both ends and is manufactured by michael corporation, and 100% by mass of solid content were further added to the adhesive solution of example 1 as a silicone resin (R3) used in the addition reaction type silicone adhesive, and the thickness of the adhesive layer 3 after drying was set to 30 μm.
Comparative example 3
An adhesive tape 1 having a total thickness of 78 μm after drying was obtained in the same manner as in example 1 except that an addition reaction type silicone adhesive comprising an organopolysiloxane having a vinylsilyl group as a silicon atom-bonded alkenyl group in the molecule was used, and an unadditized crosslinking agent type (solid content concentration: 60% by mass) SD4586 (trade name) manufactured by Torren Corning corporation was used, and the thickness of the adhesive layer 3 after drying was 40 μm.
Comparative example 4
Toluene, 166.67 parts BY mass of an addition reaction type silicone-based adhesive composed of an organopolysiloxane having a vinylsilyl group as an alkenyl group to which a silicon atom is bonded in the molecule (an unadditized crosslinking agent type of SD4584 (trade name) manufactured BY tokyo kangning corporation, solid content concentration 60 mass%), and 3.30 parts BY mass of a crosslinking agent composed of an organopolysiloxane having a hydrosilyl group in the molecule (BY 24-741 (trade name) manufactured BY tokyo kangning corporation, solid content concentration 20 mass%) were mixed and stirred. Subsequently, 6.00 parts by mass of a platinum metal catalyst (NC-25 (trade name), 25% by mass of solid content, manufactured by Toronto Corning Co., Ltd.) was added thereto, and the mixture was stirred to prepare an addition reaction type silicone adhesive solution.
On the other hand, a peroxide-curable silicone adhesive solution was prepared in the same manner as in example 9.
Next, the obtained addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution were mixed and stirred to prepare an adhesive mixed solution. The mixing ratio of the addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution was adjusted so that 50 parts by mass (solid content) of the peroxide curing type silicone adhesive was contained per 100 parts by mass (solid content) of the addition reaction type silicone adhesive.
Subsequently, the adhesive mixture solution was applied to a substrate 2 made of a polyethylene terephthalate (PET) film having a thickness of 38 μm, and then heated at 160 ℃ for 3 minutes to form an adhesive layer 3 having a thickness of 30 μm after drying. Thus, an adhesive tape 1 having a total thickness of 68 μm after drying was obtained.
Comparative example 5
First, an addition reaction type silicone adhesive solution was prepared in the same manner as the adhesive solution of the first embodiment of example 2.
On the other hand, toluene, 166.67 parts BY mass of a peroxide-curable silicone adhesive (BY 241-717 (trade name) BY Torreken corporation, solid content concentration 60% BY mass), and 5.00 parts BY mass of an initiator (NYPER K40 (trade name) BY Nichikoku corporation, solid content concentration 40% BY mass) comprising methyl benzoyl peroxide were mixed and stirred to prepare a peroxide-curable silicone adhesive solution.
Next, the obtained addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution were mixed and stirred to prepare an adhesive mixed solution. The mixing ratio of the addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution was adjusted so that 100 parts by mass (solid content) of the peroxide curing type silicone adhesive was contained per 100 parts by mass (solid content) of the addition reaction type silicone adhesive.
Subsequently, the adhesive mixture solution was applied to a substrate 2 made of a polyethylene terephthalate (PET) film having a thickness of 38 μm, and then heated at 160 ℃ for 3 minutes to form an adhesive layer 3 having a thickness of 20 μm after drying. Thus, an adhesive tape 1 having a total thickness of 58 μm after drying was obtained.
Comparative example 6
First, an addition reaction type silicone adhesive was prepared in the same manner as in example 1, except that an addition reaction type silicone adhesive comprising an organopolysiloxane having a vinylsilyl group as a silicon atom-bonded alkenyl group in the molecule was prepared in the same manner as in example 1, except that an unadditized crosslinking agent (solid content concentration, 60% by mass) of SD4587 (trade name) manufactured by tokyo kening co.
On the other hand, a peroxide-curable silicone adhesive solution was prepared in the same manner as in example 15.
Next, the obtained addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution were mixed and stirred to prepare an adhesive mixed solution. The mixing ratio of the addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution was adjusted so that 100 parts by mass (solid content) of the peroxide curing type silicone adhesive was contained per 100 parts by mass (solid content) of the addition reaction type silicone adhesive.
Subsequently, the adhesive mixture solution was applied to a substrate 2 made of a polyethylene terephthalate (PET) film having a thickness of 38 μm, and then heated at 160 ℃ for 3 minutes to form an adhesive layer 3 having a thickness of 20 μm after drying. Thus, an adhesive tape 1 having a total thickness of 58 μm after drying was obtained.
Comparative example 7
First, an addition reaction type silicone adhesive solution was prepared in the same manner as in comparative example 2.
On the other hand, a peroxide-curable silicone adhesive solution was prepared in the same manner as in comparative example 5.
Next, the obtained addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution were mixed and stirred to prepare an adhesive mixed solution. The mixing ratio of the addition reaction type silicone adhesive and the peroxide curing type silicone adhesive was adjusted so that 150 parts by mass (solid content) of the peroxide curing type silicone adhesive was contained per 100 parts by mass (solid content) of the addition reaction type silicone adhesive.
Subsequently, the adhesive mixture solution was applied to a substrate 2 made of a polyethylene terephthalate (PET) film having a thickness of 38 μm, and then heated at 160 ℃ for 3 minutes to form an adhesive layer 3 having a thickness of 20 μm after drying. Thus, an adhesive tape 1 having a total thickness of 58 μm after drying was obtained.
Comparative example 8
First, an addition reaction type silicone adhesive solution was prepared in the same manner as in example 13.
On the other hand, a peroxide-curable silicone adhesive solution was prepared in the same manner as in comparative example 6.
Next, the obtained addition reaction type silicone adhesive solution and the peroxide curing type silicone adhesive solution were mixed and stirred to prepare an adhesive mixed solution. The mixing ratio of the addition reaction type silicone adhesive and the peroxide curing type silicone adhesive was adjusted so that 30 parts by mass (solid content) of the peroxide curing type silicone adhesive was contained per 100 parts by mass (solid content) of the addition reaction type silicone adhesive.
Subsequently, the adhesive mixture solution was applied to a substrate 2 made of a polyethylene terephthalate (PET) film having a thickness of 38 μm, and then heated at 160 ℃ for 3 minutes to form an adhesive layer 3 having a thickness of 20 μm after drying. Thus, an adhesive tape 1 having a total thickness of 58 μm after drying was obtained.
The contents of the components and the thicknesses of the respective layers of the adhesive agent layer 3 in examples 1 to 15 and comparative examples 1 to 8 are shown in tables 1 to 3. In tables 1 to 3, the terms "silicone gum" and "silicone resin" are abbreviated as "gum" and "resin", respectively.
[ Table 1]
[ Table 2]
[ Table 3]
2. Evaluation method
Next, a method for evaluating the adhesive tape 1 will be described.
(1) Adhesion test
For the adhesive tapes 1 produced in examples 1 to 15 and comparative examples 1 to 8, a BA-SUS adhesion test (peel adhesion test) was performed according to the method described in the adhesive tape/sheet test method (JIS Z0237 (2009)).
Specifically, the pressure-sensitive adhesive tape 1 was adhered to a stainless steel plate (SUS304) having a surface roughness (Ra) of 50. + -.25 nm which had been subjected to a Bright Annealing (BA) treatment, and a roll having a mass of 2000g was reciprocated 1 time at a speed of 5mm/s, and pressure-bonded. Then, after leaving for 20 to 40 minutes, the plate was peeled off at a speed of 5mm/s in a direction 180 degrees from the stainless steel plate using a tensile tester, and the adhesion to the SUS plate was measured.
The adhesive tape 1 before being irradiated with ultraviolet rays was also subjected to an adhesion test. In addition, as a result of the adhesion test, if considering the fixing force when the adhesive tape 1 is used for dicing a semiconductor material, it is preferably 2.4N/10mm or more and 5.5N/10mm or less.
(2) Ball tack test
(2-1) measurement of initial ball tack
The adhesive tapes 1 produced in examples 1 to 15 and comparative examples 1 to 8 were subjected to a ball tack test according to the method described in the adhesive tape/sheet test method (JIS Z0237 (2009)).
(2-2) measurement of ball tack after UV irradiation
The adhesive layer 3 of each of the adhesive tapes 1 prepared in examples 1 to 15 and comparative examples 1 to 8 was bonded to a fluorine-based release film (SS 1A manufactured by NIPPA corporation, thickness 75 μm). Subsequently, the base material 2 side of the adhesive tape 1 was irradiated with ultraviolet rays, and left to stand at 23 ℃ and a humidity of 50 ± 5% RH for 20 to 40 minutes, and then a ball tack test was performed in the same manner as the initial ball tack according to the method described in the adhesive tape/sheet test method (JIS Z0237 (2009)).
With respect to the irradiation of ultraviolet rays, a high-pressure mercury lamp was used, and the wavelength was adjusted to 365nm so that the cumulative quantity of light was 1200mJ/cm2The irradiation is performed. Incidentally, the cumulative light amount was set to 3000mJ/cm2The ball tack was measured in the same manner as in the case of the above, but the cumulative light amount was not observed at 1200mJ/cm2Difference in time, therefore, the cumulative light amount is set to 1200mJ/cm here2Evaluation was carried out.
As a result of the ball tack test, if the pick-up property of the semiconductor chip or the like singulated by dicing is considered, the post-UV irradiation ball tack (ball number) is preferably lower than the initial ball tack (ball number).
(3) Holding force test
(3-1) measurement of initial holding force
The adhesive tapes 1 produced in examples 1 to 15 and comparative examples 1 to 8 were subjected to a holding force test according to the method described in the adhesive tape/sheet test method (JIS Z0237 (2009)).
Specifically, the adhesive tape 1 was adhered to a stainless steel plate (SUS304) polished with a water-resistant polishing paper, and held at 40 ℃ and a humidity of 33% RH while being attached with a predetermined weight, and the elapsed time (drop time (minutes)) until the adhesive tape 1 was peeled off from the stainless steel plate and dropped was measured. Further, the failure mode of the adhesive tape 1 when peeled from the stainless steel plate (whether the failure mode between the adhesive agent layer 3 and the stainless steel plate was interfacial peeling or cohesive failure) was observed. The drop time in the retention test was measured up to 5000 minutes. The dropping time (minutes) and the mode of breakage of the adhesive tape 1 are shown as the results of the holding force tests shown in tables 4 to 6 described later. The case where the adhesive tape 1 did not peel (fall) until 5000 minutes was referred to as "hold".
(3-2) measurement of Retention force after UV irradiation
The adhesive tape 1 was irradiated with ultraviolet rays in the same manner as the conditions described in the measurement of the ball tack after the UV irradiation, and after leaving, the holding force test was performed in the same manner as the initial holding force.
(3-3) relationship between holding force and failure mode
Here, the relationship between the holding force of the adhesive tape 1 and the failure mode will be described. Fig. 3 is a schematic diagram showing the relationship between the crosslink density of the addition reaction type silicone adhesive in the adhesive layer 3 and the result of the holding force test (falling time) of the adhesive tape 1.
As shown in fig. 3, in the adhesive tape 1, as the crosslinking density of the addition reaction type silicone adhesive in the adhesive layer 3 increases, the failure mode of the adhesive tape 1 in the holding power test with respect to the stainless steel plate changes in accordance with [ cohesive failure (falling) of the adhesive layer 3) ] → [ retention (non-falling) ] → [ interfacial peeling (falling) of the adhesive layer 3 and the stainless steel plate ].
As shown in fig. 3, in the region where the mode of failure of the adhesive tape 1 is cohesive failure, the holding force (fall time) of the adhesive tape 1 increases as the crosslink density of the addition reaction type silicone adhesive in the adhesive layer 3 increases.
On the other hand, as shown in fig. 3, in a region where the mode of failure of the adhesive tape 1 is interfacial peeling, the holding force (fall time) of the adhesive tape 1 decreases as the crosslink density of the addition reaction type silicone adhesive in the adhesive layer 3 increases. This is presumably because, as the crosslinking density of the addition reaction type silicone adhesive increases, the cohesive force of the adhesive layer 3 increases, the adhesive force of the adhesive tape 1 decreases, and as a result, the adhesive tape 1 is easily peeled off from the stainless steel plate and falls.
As a result of the holding power test, it is preferable that at least the failure mode after UV irradiation is holding or interface peeling, more preferable that at least the failure mode after UV irradiation is interface peeling, and further preferable that both the failure mode initially (before UV irradiation) and the failure mode after UV irradiation are interface peeling. In the case where the interface peeling is performed in both the initial (before UV irradiation) and post-UV irradiation failure modes, the retention force (fall time) after UV irradiation is preferably lower than that of the initial (before UV irradiation).
In this case, when the adhesive tape 1 is used for dicing a semiconductor element substrate or the like and then the obtained semiconductor chip or the like is peeled off from the adhesive tape 1, UV is irradiated to the adhesive tape 1, and thus the semiconductor chip or the like is less likely to have adhesive residue.
(4) Residual gum test on organic silicon resin
The adhesive tapes 1 produced in examples 1 to 15 and comparative examples 1 to 8 were subjected to a residual adhesive test for a silicone resin.
First, an agent a and an agent B of a methyl group-containing silicone resin (KER-2500N (trade name) manufactured by shin-Etsu chemical Co., Ltd.) as a silicone resin for LED devices were mixed in a mixing ratio of 1: 1 to prepare a mixed solution. This mixed solution was applied to a stainless steel plate, and cured by heating at 100 ℃ for 1 hour and further at 150 ℃ for 2 hours to prepare a silicone test piece a.
Similarly, agent a and agent B of a phenyl group-containing silicone resin (KER-6110 (trade name) manufactured by shin-Etsu chemical Co., Ltd.) as a silicone resin for LED devices were mixed in a mixing ratio of 3: 7 to prepare a mixed solution. This mixed solution was applied to a stainless steel plate, and cured by heating at 100 ℃ for 2 hours and further at 150 ℃ for 5 hours to prepare a silicone test piece B.
Subsequently, the adhesive layers 3 of the adhesive tapes 1 were respectively stuck to the silicone test pieces A, B, and pressure-bonded by reciprocating a roller having a mass of 2000g 1 time at a speed of 5 mm/s. Subsequently, ultraviolet rays were irradiated from the base material 2 side of the pressure-sensitive adhesive tape 1 in the same manner as the conditions described in the measurement of the ball tack after UV irradiation, and then the pressure-sensitive adhesive tape was left for 120 hours in an atmosphere of 40 ℃ and 90% RH. Then, the adhesive tape 1 was peeled off at a speed of 800mm/s to 1200mm/s at room temperature in a direction of 90 ° from the silicone test piece A, B, and the residue of the silicone test piece A, B was visually confirmed.
(5) Residual epoxy resin test
The adhesive tapes 1 produced in examples 1 to 15 and comparative examples 1 to 8 were subjected to a residual adhesive test for an epoxy resin.
An epoxy test piece comprising an epoxy resin plate (NL-EG-23 (trade name) manufactured by Nisshinoka chemical Co., Ltd.) obtained by impregnating a glass cloth substrate with an epoxy resin was bonded with the adhesive layer 3 of the adhesive tape 1, and the tape was pressure-bonded by reciprocating a roll having a mass of 2000g 1 time at a speed of 5 mm/s. Subsequently, ultraviolet rays were irradiated from the base material 2 side of the pressure-sensitive adhesive tape 1 in the same manner as the conditions described in the measurement of the ball tack after UV irradiation, and then the pressure-sensitive adhesive tape was left for 120 hours in an atmosphere of 40 ℃ and 90% RH. Then, the adhesive tape 1 was peeled off at a speed of 800mm/s to 1200mm/s at room temperature in a direction of 90 ° from the epoxy test piece, and the residual adhesive on the epoxy test piece was visually confirmed.
The silicone resin cull test and the epoxy resin cull test were evaluated according to the following criteria. The evaluation of a or B was defined as pass.
A: no adhesive residue in the range of 100% per unit area of the test piece
B: cull was observed in the range of less than 2% per unit area of the test piece
C: the residual gum was observed in the range of 2% or more and less than 5% per unit area of the test piece
D: the adhesive residue was observed in the range of 5% or more per unit area of the test piece, or in the edge portion of the test piece
(6) Cutting test
The adhesive tapes 1 produced in examples 1 to 15 and comparative examples 1 to 8 were subjected to a cutting test.
Specifically, first, an epoxy resin for molding (CEL-400 ZHF40-W75G (trade name) manufactured by Hitachi chemical Co., Ltd.) was charged into a mold and sealed at a sealing pressure of 50kgf/cm2(491N/cm2) The sealant was heated and cured at a thickness of 0.3mm and a heating temperature of 150 ℃ for 300 seconds to prepare a cut test piece in the form of a disk (200 mm (8 inches) in diameter).
The adhesive layer 3 of the adhesive tape 1 was attached to a dicing ring, and the portion that had oozed out of the ring was cut off, and then the cut portion was further bonded to a fluorine-based release film (product name, SS1A manufactured by NIPPA corporation, thickness 75 μm). Subsequently, a roller having a mass of 2000g was reciprocated to press the adhesive tape 1 against the loop portion. Subsequently, the fluorine-based release film was peeled off, and the dicing test piece was bonded to the adhesive layer in the center portion of the ring and pressure-bonded.
Further, the dicing test piece was cut into chips of 10mm × 10mm together with the adhesive tape 1 by using a dicing blade manufactured by Disco, Ltd, using a dicing apparatus (A-WD-100A (trade name)) manufactured by Tokyo precision Co. At this time, the number of scattered chips was measured, and the fixing force in the dicing test was evaluated.
Subsequently, the pressure-sensitive adhesive tape 1 adhered to the chip singulated into pieces of 10mm × 10mm was irradiated with ultraviolet rays in the same manner as the conditions described in the measurement of the ball tack after UV irradiation. Then, the singulated chips were picked up from the adhesive tape 1, and the presence or absence of adhesive residue on the chips was visually checked, and the adhesive residue was evaluated in the dicing test. In addition, the number of chips that failed in picking up the chips was measured, and the picking-up property in the dicing test was evaluated.
The holding force in the cutting test was evaluated according to the following criteria. The evaluation of a or B was defined as pass.
A: the number of scattered chips was 0 out of 100
B: the number of scattered chips was 1 out of 100
C: the number of scattered chips was 2 out of 100
D: the number of scattered chips is 3 or more out of 100
The residual gum in the cutting test was evaluated according to the following criteria. Note that the evaluation of a is regarded as pass.
A: no adhesive residue was observed on the chip
D: residual glue was observed on the chip, or stringing of the adhesive was observed on the side of the chip
The pick-up property in the cutting test was evaluated according to the following criteria. The evaluation of a or B was defined as pass.
A: the number of chips failing in pickup was 0 out of 100
B: the number of chips failing in pickup was 1 out of 100
C: the number of chips failing in pickup was 2 out of 100
D: the number of chips failing in pickup is 3 or more out of 100
3. Test results
The evaluation results of the adhesive tapes 1 of examples 1 to 15 and comparative examples 1 to 8 are shown in tables 4 to 6.
[ Table 4]
[ Table 5]
[ Table 6]
As shown in tables 4 to 6, it was confirmed that: in the adhesive tapes 1 of examples 1 to 8 in which the adhesive layer 3 is based on an addition reaction type silicone adhesive and contains a photosensitive platinum (Pt) catalyst and a crosslinking agent for the addition reaction type silicone adhesive, and the adhesive tapes 1 of examples 9 to 15 in which the adhesive layer 3 is based on a mixture of an addition reaction type silicone adhesive and a peroxide curing type silicone adhesive and contains a photosensitive platinum (Pt) catalyst and a crosslinking agent for the addition reaction type silicone adhesive, the adhesive force test, the ball tack test, the holding force test, the silicone resin residual glue test, the epoxy resin residual glue test, and the cutting test (fixing force, residual glue, and pick-up property) were satisfactory results.
Thus, it was confirmed that: the adhesive tapes 1 of examples 1 to 8 in which the adhesive layer 3 is based on an addition reaction type silicone adhesive and contains a photosensitive platinum (Pt) catalyst and a crosslinking agent for the addition reaction type silicone adhesive, and the adhesive tapes 1 of examples 9 to 15 in which the adhesive layer 3 is based on a mixture of an addition reaction type silicone adhesive and a peroxide curing type silicone adhesive and contains a photosensitive platinum (Pt) catalyst and a crosslinking agent for the addition reaction type silicone adhesive are useful as dicing adhesive tapes for semiconductor materials, more specifically, dicing adhesive tapes for dicing which are bonded from the sealing resin side of a semiconductor element substrate.
In contrast, it was confirmed that: in comparative examples 1 to 3 in which the adhesive layer 3 does not satisfy the condition of the adhesive layer 3 of the first embodiment and comparative examples 4 to 8 in which the adhesive layer 3 does not satisfy the condition of the adhesive layer 3 of the second embodiment, all the test results are inferior to those in examples 1 to 15 in the silicone resin residue test, the epoxy resin residue test, and the cutting test (fixing force, residue, and pickup property).
Specifically, in the adhesive tape 1 of comparative example 1 in which the photosensitive platinum (Pt) catalyst is not contained in the adhesive agent layer 3 of the first embodiment, although a normal platinum (Pt) catalyst is contained, the results of the ball tack test and the holding power test are not changed before and after UV irradiation, and the cohesive force is not sufficiently improved, so that a large amount of cull is observed in the silicone resin cull test and the epoxy resin cull test. In the dicing test, the chip obtained by dicing the test piece had poor pick-up properties, and adhesive residue was observed on the chip.
The same results as in comparative example 1 were obtained also in the adhesive tape 1 of comparative example 4 in which the photosensitive platinum (Pt) catalyst was not contained in the adhesive agent layer 3 of the second embodiment.
Further, in the adhesive tape 1 of comparative example 2 in which the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) to the total mass (Rw) of the silicone resin (R) and the content ratio of the silicone gum (G1) having an alkenyl group in the total mass of the silicone gum (G) and the silicone resin (R) are respectively less than the lower limit value of the adhesive layer 3 of the first embodiment, the adhesive force was high, the change in the results of the ball tack test and the holding power test before and after UV irradiation was small, and the cohesive force was slightly insufficiently improved. Therefore, in the tests on silicone resin cull and on epoxy resin cull, a large amount of cull was observed. In the dicing test, the chip obtained by dicing the test piece had poor pick-up properties, and adhesive residue was observed on the chip surface.
Further, in the adhesive tape 1 of comparative example 3 in which the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) to the total mass (Rw) of the silicone resin (R) and the content ratio of the silicone gum (G1) having an alkenyl group in the total mass of the silicone gum (G) and the silicone resin (R) each exceed the upper limit value of the adhesive layer 3 of the first embodiment, although the results of the ball tack test and the holding power test varied before and after UV irradiation, the cohesive force increased, but the adhesive force was low, so that the fixing force of the cut test piece was low in the cutting test, and scattering of a large number of chips was observed. Note that no cull was observed in the cull to silicone test and the cull to epoxy test. In addition, no adhesive residue was observed in the dicing test for the non-scattering chips.
Further, it is found that the adhesive tape 1 of comparative example 5, in which the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) to the total mass (Rw) of the silicone resin (R) is less than the lower limit of the adhesive layer 3 of the second embodiment, has a slightly changed result of the ball tack test and the holding power test before and after UV irradiation, and improves the cohesive force, but it cannot be said that this is sufficient, and the chip pickup property of the cut test piece is slightly poor in the dicing test. Note that, in the silicone resin cull test and the epoxy resin cull test, a small amount of cull was observed, and in the dicing test, no cull was observed for chips that could be picked up.
Further, in the adhesive tape 1 of comparative example 6 in which the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) to the total mass (Rw) of the silicone resin (R) exceeds the upper limit value of the adhesive layer 3 of the second embodiment, although the results of the ball tack test and the holding power test varied before and after UV irradiation and the cohesive force was improved, the adhesive force was low, and therefore, in the dicing test, the fixing force of the dicing test piece was low and scattering of a large number of chips was observed. Note that no cull was observed in the cull to silicone test and the cull to epoxy test. In addition, no adhesive residue was observed in the dicing test for the non-scattering chips.
Further, in the adhesive tape 1 of comparative example 7 in which the mass ratio (Gw)/(Rw) of the total mass (Gw) of the silicone gum (G) to the total mass (Rw) of the silicone resin (R) exceeds the upper limit value of the adhesive layer 3 of the second embodiment, and the content ratio of the silicone gum (G1) having an alkenyl group in the total mass of the silicone gum (G) and the silicone resin (R) is less than the lower limit value of the adhesive layer 3 of the second embodiment, the adhesive force is high due to the influence of the curing of the peroxide-curable silicone adhesive, and the results of the ball tack test and the holding force test before and after UV irradiation change little, and further improvement of the cohesive force is slightly insufficient. Therefore, in the tests on silicone resin cull and on epoxy resin cull, a large amount of cull was observed. In the dicing test, the chip obtained by dicing the test piece had poor pick-up properties, and adhesive residue was observed on the chip surface.
Further, in the adhesive tape 1 of comparative example 8 in which the content ratio of the silicone rubber compound (G1) having an alkenyl group in the total mass of the silicone rubber compound (G) and the silicone resin (R) exceeds the upper limit value of the adhesive layer 3 of the second embodiment, although the results of the ball tack test and the holding power test varied before and after UV irradiation and the cohesive force was improved, the adhesive force was low, and therefore, the fixing force of the dicing test piece was low in the dicing test and scattering of a large number of chips was observed. Note that no cull was observed in the cull to silicone test and the cull to epoxy test. In addition, no adhesive residue was observed in the dicing test for the non-scattering chips.
Description of the symbols
1: adhesive tape, 2: base material, 3: adhesive layer, 100: semiconductor element substrate, 101: substrate, 102: semiconductor element, 103: sealing resin, 200: a semiconductor chip.
Claims (6)
1. An adhesive tape for dicing, characterized in that,
which comprises a base material and a silicone adhesive layer laminated on the base material, and is used for dividing a semiconductor material having a plurality of semiconductor elements covered with a coating material into a plurality of semiconductor chips,
the silicone adhesive layer uses an addition reaction type silicone adhesive as a main agent, and contains a photosensitive platinum (Pt) catalyst and a crosslinking agent for the addition reaction type silicone adhesive,
the mass ratio Gw/Rw of the total mass Gw of the silicone rubber G contained in the silicone adhesive layer to the total mass Rw of the silicone resin R is in the range of 35/65-50/50, the content ratio of the silicone rubber G1 having an alkenyl group in the total mass of the silicone rubber G and the silicone resin R is in the range of 35-50% by mass,
the adhesive tape for dicing satisfies all of the following conditions (a) to (c) in adhesive properties according to JIS Z0237 (2009):
(a) the adhesive force to a BA-SUS test plate before light irradiation is 2.4N/10mm or more and 5.5N/10mm or less,
(b) the ball number in the tilt ball viscosity test at a tilt angle of 30 DEG, a temperature of 23 ℃ and a relative humidity of 50% RH is in the relationship of BN0 > BN1 when the ball number before light irradiation is BN0 and the ball number after light irradiation is BN1,
(c) in the retention test after light irradiation at a temperature of 40 ℃, a relative humidity of 33% RH and a leaving time of 5000 minutes, the phenomenon of breakage at the time of dropping means that the silicone adhesive layer peels off from the interface with the BA-SUS test plate or does not drop in the retention test.
2. The adhesive tape for dicing according to claim 1, wherein the semiconductor material in which the plurality of semiconductor elements are sealed with the coating material made of silicone resin is used by being stuck from the coating material side.
3. An adhesive tape for dicing, characterized in that,
which comprises a base material and a silicone adhesive layer laminated on the base material, and is used for dividing a semiconductor material having a plurality of semiconductor elements covered with a coating material into a plurality of semiconductor chips,
the silicone adhesive layer comprises a mixture of an addition reaction type silicone adhesive and a peroxide curing type silicone adhesive as a main agent, and comprises a photosensitive platinum (Pt) catalyst and a crosslinking agent for the addition reaction type silicone adhesive,
the mass ratio Gw/Rw of the total mass Gw of the silicone rubber G contained in the silicone adhesive layer to the total mass Rw of the silicone resin R is in the range of 40/60-56/44, the content ratio of the silicone rubber G1 having an alkenyl group in the total mass of the silicone rubber G and the silicone resin R is in the range of 14-42% by mass,
the adhesive tape for dicing satisfies all of the following conditions (a) to (c) in the adhesive properties according to JIS Z0237 (2009):
(a) the adhesive force to a BA-SUS test plate before light irradiation is 2.4N/10mm or more and 5.5N/10mm or less,
(b) the ball number in the tilt ball viscosity test at a tilt angle of 30 DEG, a temperature of 23 ℃ and a relative humidity of 50% RH is in the relationship of BN0 > BN1 when the ball number before light irradiation is BN0 and the ball number after light irradiation is BN1,
(c) in the retention test after light irradiation at a temperature of 40 ℃, a relative humidity of 33% RH and a leaving time of 5000 minutes, the phenomenon of breakage at the time of dropping means that the silicone adhesive layer peels off from the interface with the BA-SUS test plate or does not drop in the retention test.
4. The adhesive tape for dicing according to claim 3, wherein the semiconductor material in which the plurality of semiconductor elements are sealed with the coating material made of silicone resin is used by being stuck from the coating material side.
5. The adhesive tape for dicing according to claim 3 or 4, wherein the silicone-based adhesive layer further contains an initiator composed of a peroxide.
6. A method for manufacturing a semiconductor chip includes the steps of:
a bonding step of bonding the adhesive tape for dicing according to any one of claims 1 to 5 to a semiconductor element substrate having a plurality of semiconductor elements formed on the substrate and sealed with a sealing resin made of a silicone resin, from the sealing resin side;
a cutting step of cutting the semiconductor element substrate to which the dicing adhesive tape is attached into a plurality of semiconductor chips;
an irradiation step of irradiating the dicing adhesive tape of the semiconductor element substrate with light; and
a peeling step of peeling the dicing adhesive tape from the plurality of semiconductor chips.
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| JP2018-164411 | 2018-09-03 | ||
| PCT/JP2019/034126 WO2020050167A1 (en) | 2018-09-03 | 2019-08-30 | Adhesive tape for dicing and method for manufacturing semiconductor chips |
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| KR (1) | KR102632461B1 (en) |
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| CN113320036A (en) * | 2021-06-18 | 2021-08-31 | 常州时创能源股份有限公司 | Cutting process for strip silicon material and application thereof |
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| KR20220116184A (en) * | 2019-12-19 | 2022-08-22 | 맥셀 주식회사 | Manufacturing method of adhesive tape for dicing and semiconductor chip |
| CN114868229A (en) * | 2019-12-20 | 2022-08-05 | 麦克赛尔株式会社 | Adhesive tape for dicing and method for manufacturing semiconductor chip |
| CN115485814A (en) | 2020-04-30 | 2022-12-16 | 信越化学工业株式会社 | Temporary adhesive for wafer processing, wafer laminate, and method for producing thin wafer |
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| JP2015050216A (en) * | 2013-08-30 | 2015-03-16 | 日立マクセル株式会社 | Adhesive tape for dicing and method of manufacturing semiconductor chip |
| CN105733462A (en) * | 2014-12-25 | 2016-07-06 | 日立麦克赛尔株式会社 | Adhesive tape for dicing and method of manufacturing semiconductor chip |
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| JP2005093503A (en) | 2003-09-12 | 2005-04-07 | Hitachi Cable Ltd | Dicing method |
| JP2013038408A (en) | 2011-07-14 | 2013-02-21 | Nitto Denko Corp | Adhesive tape for fixing semiconductor wafer, method for manufacturing semiconductor chip and adhesive tape with adhesive film |
| JP5880399B2 (en) | 2012-11-13 | 2016-03-09 | 信越化学工業株式会社 | Method for producing silicone rubber molding |
| KR20150112851A (en) | 2014-03-28 | 2015-10-07 | 신에쓰 가가꾸 고교 가부시끼가이샤 | Silicone adhesive composition, method for making the same and adhesive film |
| US9777203B2 (en) * | 2015-06-08 | 2017-10-03 | Momentive Performance Materials | Silicone pressure sensitive adhesive compositions and protective films containing the same |
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| JPH1095920A (en) * | 1996-09-25 | 1998-04-14 | Shin Etsu Chem Co Ltd | Photocurable liquid silicone rubber composition for impression master block |
| US5952397A (en) * | 1996-09-25 | 1999-09-14 | Shin-Etsu Chemical Co., Ltd. | Photo-curable liquid silicone rubber compositions for templating mother molds |
| JP2015050216A (en) * | 2013-08-30 | 2015-03-16 | 日立マクセル株式会社 | Adhesive tape for dicing and method of manufacturing semiconductor chip |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113320036A (en) * | 2021-06-18 | 2021-08-31 | 常州时创能源股份有限公司 | Cutting process for strip silicon material and application thereof |
| CN113320036B (en) * | 2021-06-18 | 2024-02-13 | 常州时创能源股份有限公司 | Squaring and cutting process of strip-shaped silicon material and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| KR102632461B1 (en) | 2024-02-02 |
| JP7374909B2 (en) | 2023-11-07 |
| JPWO2020050167A1 (en) | 2021-08-26 |
| TW202020094A (en) | 2020-06-01 |
| KR20210056334A (en) | 2021-05-18 |
| JP2023138530A (en) | 2023-10-02 |
| WO2020050167A1 (en) | 2020-03-12 |
| TWI799618B (en) | 2023-04-21 |
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