TW202111072A - Silicone composition for die bonding, cured product thereof and optical semiconductor device - Google Patents

Abstract

Provided is a silicone composition for die bonding, which imparts a cured product having excellent hardness and chip shear strength and suppresses contamination of a metal gasket in an optical semiconductor device. The silicone composition for die bonding contains, at a specific blending ratio, a silicone resin; (A) An organopolysiloxane which contains two or more alkenyl groups per molecule and has a viscosity of 100 mPas or less at 25 DEG C; (B) a specific three-dimensional network organopolysiloxane that is wax-like or solid at 23 DEG C; (C) a specific organohydrogenpolysiloxane having at least two hydrogen atoms bonded to a silicon atom in one molecule; (D) a specific polysiloxane containing an epoxy group; and (E) a platinum group metal-based catalyst.

Description

Polysilicon oxide composition for die bonding, its hardened product and optical semiconductor device

The present invention relates to a polysilicon oxide composition for die bonding, a cured product thereof, and an optical semiconductor device using the cured product.

Recently, the sealing material and die bonding material of light-emitting diode (hereinafter referred to as "LED") components have increased heat generation due to the increase in the brightness of LED components. Therefore, the use of silicone resin with good durability (patented) Literature 1, 2). Especially when the resin in the die-bonding material is too soft, in the wire bonding step performed after the die-bonding step, the defect that bonding cannot be performed occurs, so a die-bonding material with high hardness is required.

In addition, LED devices have progressed in miniaturization in recent years, and die-bonding materials with higher adhesion are required. When the bonding force of the die-bonding material is insufficient, chip peeling may occur during the wire bonding step in LED manufacturing, which becomes a fatal problem on the manufacturing surface. Although the polysilicone bonded crystal materials have excellent durability, the adhesiveness is insufficient, and materials with higher grain shear strength are desired.

In addition to the high grain shear strength, there are also cases where the low-molecular components generated during the heating and hardening of the die-bonding material contaminate the gold pad of the chip, which will become the cause of the shortcomings in the wire bonding step. Although polysiloxanes use silane coupling agents with adhesive functional groups in order to improve adhesion, generally silane coupling agents are of low molecular weight and will volatilize when the heat (100~180℃) is applied during the hardening step of the die. Porosity occurs or the shear strength of the crystal grains is reduced, which is the cause of the contamination of the gold pad. That is, it is desired to increase the shear strength of the die without contamination of the gold pad. [Prior Technical Literature] [Patent Literature]

[Patent Document 1] JP 2006-342200 A [Patent Document 2] JP 2010-285571 A

[The problem to be solved by the invention]

The present invention was completed in view of the above circumstances, and its object is to provide a polysilicon oxide composition for die bonding that can impart a cured product with excellent hardness and die shear strength and suppressed contamination of the gold pad in an optical semiconductor device. [Means to solve the problem]

(式中，R¹ 分別為相同或不同，不含烯基之取代或非取代一價烴基，R² 分別為相同或不同之烯基，a、b、c、d、e、f、g及h分別為滿足a≧0、b≧0、c≧0、d≧0、e≧0、f≧0、g≧0及h≧0之數，但係滿足b+c＞0，f+g+h＞0且a+b+c+d+e+f+g+h=1之數) (C)以下述平均組成式(2)表示，1分子中具有至少2個鍵結於矽原子之氫原子之有機氫聚矽氧烷：相對於(A)成分及(B)成分中之全部鍵結於矽原子之烯基之合計數，(C)成分中之鍵結於矽原子之氫原子之數成為0.5~5.0倍之量，

(式中，R¹ 與前述相同，i及j係滿足0.7≦i≦2.1、0.001≦j≦1.0且0.8≦i+j≦3.0之數) (D)以下述式(3)表示之含有環氧基之聚矽氧烷：相對於(A)成分、(B)成分及(C)成分之合計100質量份為1~25質量份，

(式中，R¹ 與前述相同，R³ 分別為相同或不同之含環氧基之基，R⁴ 分別相同或不同為不含烯基之取代或非取代之一價烴基，k及m分別為滿足k＞0、m≧0及k+m=1之數，n係滿足0≦n≦2之數)， (E)鉑族金屬系觸媒：相對於(A)成分、(B)成分、(C)成分及(D)成分之合計質量，以鉑屬金屬元素之質量換算為1~500ppm。In order to achieve the above-mentioned problems, the present invention provides a polysilicon oxide composition for crystal bonding containing the following (A) components to (E) components. (A) Organopolysiloxane with 2 or more alkenyl groups in one molecule and a viscosity of 100 mPa･s or less at 25°C, (B) represented by the following formula (1), waxy at 23°C Or solid three-dimensional network organopolysiloxane: 70 to 95 parts by mass relative to 100 parts by mass of the total of (A) component and (B) component,

(In the formula, R ¹ are the same or different substituted or unsubstituted monovalent hydrocarbon groups without alkenyl, R ² are the same or different alkenyl groups, a, b, c, d, e, f, g and h is the number that satisfies a≧0, b≧0, c≧0, d≧0, e≧0, f≧0, g≧0, and h≧0, but satisfies b+c>0, f+g +h＞0 and a+b+c+d+e+f+g+h=1) (C) is represented by the following average composition formula (2), and there are at least two silicon atoms in one molecule The organohydrogen polysiloxane of hydrogen atoms: relative to the total number of alkenyl groups bonded to silicon atoms in the components (A) and (B), the hydrogen bonded to silicon atoms in the component (C) The number of atoms becomes 0.5~5.0 times the amount,

(In the formula, R ¹ is the same as the above, i and j are the numbers satisfying 0.7≦i≦2.1, 0.001≦j≦1.0, and 0.8≦i+j≦3.0) (D) Containing ring represented by the following formula (3) Polysiloxane of oxy group: 1-25 parts by mass relative to 100 parts by mass of the total of (A) component, (B) component and (C) component,

(In the formula, R ¹ is the same as above, R ³ is the same or different epoxy-containing group, R ^{4 is the} same or different, is a substituted or unsubstituted monovalent hydrocarbon group without alkenyl, k and m are respectively In order to satisfy the number of k>0, m≧0 and k+m=1, the n system satisfies the number of 0≦n≦2), (E) platinum group metal catalyst: relative to (A) component, (B) The total mass of components, (C) components, and (D) components is 1 to 500 ppm in terms of the mass of platinum metal elements.

According to the polysilicon oxide composition for die bonding of the present invention, it is possible to impart a hardened product with excellent hardness and die shear strength and suppressed contamination of the gold pad in the optical semiconductor device.

(式中，R¹ 及R² 與前述相同，o、p、q、r分別為滿足q≧0、r≧0、o≧0、p≧0之數，但係滿足q+r＞0、r+o＞0、o+p＞0且o+p+q+r=1之數)。The aforementioned component (A) is preferably an organopolysiloxane represented by the following formula (4),

(In the formula, R ¹ and R ^{2 are the} same as above, o, p, q, r are the numbers satisfying q≧0, r≧0, o≧0, p≧0, but satisfying q+r>0, r+o>0, o+p>0 and o+p+q+r=1).

If the aforementioned component (A) is an organopolysiloxane with the aforementioned characteristics, the polysiloxane composition for die bonding can impart more excellent hardness and die shear strength, and the contamination of the gold pad in the optical semiconductor device is more suppressed. Hardened objects.

In the aforementioned formula (1), b>0 and h>0 are preferred. In the aforementioned formula (1), if b>0 and h>0, the polysilicon oxide composition for die bonding becomes more excellent in imparting hardness and grain shear strength, and in particular, imparting bonding strength and gold bonding in optical semiconductor devices. Those with hardened materials whose mat pollution is more restrained.

The aforementioned component (C) preferably has a mass reduction of 1% by mass or less when heated at 150°C for 30 minutes under 1 atmosphere. If the aforementioned component (C) is the aforementioned one, the polysilicon oxide composition for die bonding will be the one in which the contamination of the gold pad in the optical semiconductor device is more suppressed.

The aforementioned component (D) preferably has a mass reduction of 5% by mass or less when heated at 150°C for 30 minutes under 1 atmosphere. If the aforementioned component (D) is the aforementioned one, the polysilicon oxide composition for die bonding will be more suppressed in the contamination of the gold pad in the optical semiconductor device.

(式中，s為1~6之整數，虛線表示鍵結鍵)。In the aforementioned component (D), R ³ is preferably a group represented by the following formula (5),

(In the formula, s is an integer from 1 to 6, and the dashed line represents the bonding bond).

If R ³ is the aforementioned specific functional group, the polysiloxane composition for die bonding becomes a hardened product that can impart more excellent hardness and die shear strength, and can more suppress the contamination of the gold pad in the optical semiconductor device.

In the aforementioned composition, it is preferable that more than 80 mol% of ^{all R 1 are methyl groups.} If 80 mol% or more of all R ¹ in the aforementioned composition is methyl, the polysiloxane composition for die bonding can impart heat resistance, light resistance (ultraviolet resistance), and stress against heat and ultraviolet rays. A cured product with excellent resistance to deterioration such as discoloration.

The aforementioned composition preferably contains (F) fumed silica having a BET specific surface area of 100 to 400 m ² /g. If the composition contains the fumed silica, the composition has excellent thixotropy and workability.

The present invention also provides a cured polysilicone, which is a cured product of the aforementioned polysilicone composition for crystal bonding. According to this polysiloxy hardened product, it has excellent hardness and die shear strength, and has high adhesion to substrates, LED chips, etc., and can be especially used as a die bonding material for die bonding of LED components.

Furthermore, the present invention provides an optical semiconductor device, which is obtained by bonding an optical semiconductor element with the aforementioned polysiloxy hardened material. According to this type of optical semiconductor device, since the aforementioned cured polysilicon oxide is used as a die bonding material that has excellent hardness and die shear strength, and has high adhesion to substrates, LEDs, etc., it is highly reliable. [Effects of the invention]

As mentioned above, the polysilicon oxide composition for die bonding according to the present invention can provide hardened products with excellent hardness and die shear strength and suppressed contamination of gold pads in optical semiconductor devices, so it is used as a bonding agent for LED devices, etc. The bonding material used for the crystal is particularly useful. Moreover, in the wire bonding step performed after the die bonding step, the defects such as chip peeling and inability to bond the die are difficult to occur. The optical semiconductor device using the polysilicon oxide hardening material to bond the optical semiconductor element to the die has high reliability, and its production Sex is also improved.

As mentioned above, it is required to develop a die-bonding material for die bonding of LED devices with less contamination by gold pads, and a polysilicone composition for die-bonding that can impart a polysilicon cured product with excellent hardness and die shear strength.

The inventors of the present invention have repeatedly actively reviewed the above-mentioned issues and found that if it is a polysilicone composition for crystal bonding that includes the following components (A), (B), (C), (D) and (E), it can be achieved The above-mentioned problems have led to the completion of the present invention.

(式中，R¹ 分別為相同或不同，不含烯基之取代或非取代一價烴基，R² 分別為相同或不同之烯基，a、b、c、d、e、f、g及h分別為滿足a≧0、b≧0、c≧0、d≧0、e≧0、f≧0、g≧0及h≧0之數，但係滿足b+c＞0，f+g+h＞0且a+ b+c+d+e+f+g+h=1之數)， (C)以下述平均組成式(2)表示，1分子中具有至少2個鍵結於矽原子之氫原子之有機氫聚矽氧烷：相對於(A)成分及(B)成分中之全部鍵結於矽原子之烯基之合計數，(C)成分中之鍵結於矽原子之氫原子之數成為0.5~5.0倍之量，

(式中，R¹ 與前述相同，i及j係滿足0.7≦i≦2.1、0.001≦j≦1.0且0.8≦i+j≦3.0之數)， (D)以下述式(3)表示之含有環氧基之聚矽氧烷：相對於(A)成分、(B)成分及(C)成分之合計100質量份為1~25質量份，

(式中，R¹ 與前述相同，R³ 分別為相同或不同之含環氧基之基，R⁴ 分別相同或不同為不含烯基之取代或非取代之一價烴基，k及m分別為滿足k＞0、m≧0及k+m=1之數，n係滿足0≦n≦2之數)， (E)鉑族金屬系觸媒：相對於(A)成分、(B)成分、(C)成分及(D)成分之合計質量，以鉑屬金屬元素之質量換算為1~500ppm。That is, the present invention is a polysiloxane composition for crystal bonding containing the following (A) components to (E) components. (A) Organopolysiloxane with 2 or more alkenyl groups in one molecule and a viscosity of 100 mPa･s or less at 25°C, (B) represented by the following formula (1), waxy at 23°C Or solid three-dimensional network organopolysiloxane: 70 to 95 parts by mass relative to 100 parts by mass of the total of (A) component and (B) component,

(In the formula, R ¹ are the same or different substituted or unsubstituted monovalent hydrocarbon groups without alkenyl, R ² are the same or different alkenyl groups, a, b, c, d, e, f, g and h is the number that satisfies a≧0, b≧0, c≧0, d≧0, e≧0, f≧0, g≧0, and h≧0, but satisfies b+c>0, f+g +h＞0 and a+b+c+d+e+f+g+h=1), (C) is represented by the following average composition formula (2), and there are at least 2 bonding to silicon atoms in a molecule The organohydrogen polysiloxane of hydrogen atoms: relative to the total number of alkenyl groups bonded to silicon atoms in the components (A) and (B), the hydrogen bonded to silicon atoms in the component (C) The number of atoms becomes 0.5~5.0 times the amount,

(In the formula, R ¹ is the same as the above, i and j satisfy the number of 0.7≦i≦2.1, 0.001≦j≦1.0, and 0.8≦i+j≦3.0), (D) is contained in the following formula (3) Polysiloxane of epoxy group: 1-25 parts by mass relative to 100 parts by mass of the total of (A) component, (B) component and (C) component,

(In the formula, R ¹ is the same as above, R ³ is the same or different epoxy-containing group, R ^{4 is the} same or different, is a substituted or unsubstituted monovalent hydrocarbon group without alkenyl, k and m are respectively In order to satisfy the number of k>0, m≧0 and k+m=1, the n system satisfies the number of 0≦n≦2), (E) platinum group metal catalyst: relative to (A) component, (B) The total mass of components, (C) components, and (D) components is 1 to 500 ppm in terms of the mass of platinum metal elements.

The following describes the present invention in detail, but the present invention is not limited thereto. [Polysiloxane composition for die bonding] The silicone composition for crystal bonding of the present invention contains the following components (A) to (E). Each component is explained in detail below.

＜(A) Ingredient＞ (A) Component is an organopolysiloxane with two or more alkenyl groups in one molecule and a viscosity of 100 mPa･s or less at 25°C. (A) The viscosity of the component is measured with a rotary viscometer at 25° C. The value is 100mPa･s or less, preferably 30mPa･s or less. In the case of more than 100mPa･s, the viscosity of the polysiloxane composition for die bonding becomes higher, so it is difficult to handle the process in the step of coating the composition on the LED substrate by the die bonding machine. In addition, in the following, unless otherwise specified, the viscosity is the value measured with a rotary viscometer at 25°C.

The alkenyl group contained in the component (A) is not particularly limited, but it is preferably an alkenyl group having 2 to 10 carbon atoms such as a vinyl group, an allyl group, and an ethynyl group, and more preferably an alkenyl group having 2 to 6 carbon atoms. More preferably, it is vinyl.

The component (A) may be a substituted or unsubstituted monovalent hydrocarbon group that does not contain an alkenyl group. As an example, it is not particularly limited if it does not have an alkenyl group, but it is preferably substituted or unsubstituted with 1 to 8 carbon atoms A monovalent hydrocarbon group. Examples of the monovalent hydrocarbon group include alkyl groups such as methyl, ethyl, propyl, and butyl, cycloalkyl groups such as cyclohexyl and cyclopentyl, aryl groups such as phenyl, tolyl and xylyl, and benzyl Aralkyl groups such as chloromethyl, phenylethyl, etc.; halogenated hydrocarbon groups such as chloromethyl, chloropropyl, and chlorocyclohexyl. Preferably it is an alkyl group, more preferably it is a methyl group.

(式中，R¹ 分別為相同或不同，不含烯基之取代或非取代一價烴基，R² 分別為相同或不同之烯基，o、p、q、r分別為滿足q≧0、r≧0、o≧0、p≧0之數，但係滿足q+r＞0、r+o＞0、o+p＞0且o+p+q+r=1之數)。As the (A) component, a branched organopolysiloxane represented by the following average composition formula (4) is exemplified.

(In the formula, R ¹ are the same or different substituted or unsubstituted monovalent hydrocarbon groups that do not contain alkenyl groups, R ² are the same or different alkenyl groups, and o, p, q, and r are each satisfying q≧0, r≧0, o≧0, p≧0, but satisfying q+r>0, r+o>0, o+p>0 and o+p+q+r=1).

The substituted or unsubstituted monovalent hydrocarbon group not containing an alkenyl group represented by R ¹ is not particularly limited if it does not have an alkenyl group, but it is preferably a substituted or unsubstituted monovalent hydrocarbon group having 1 to 8 carbon atoms Hydrocarbyl. Examples of the monovalent hydrocarbon group include alkyl groups such as methyl, ethyl, propyl, and butyl, cycloalkyl groups such as cyclohexyl and cyclopentyl, aryl groups such as phenyl, tolyl and xylyl, and benzyl Aralkyl groups such as chloromethyl, phenylethyl, etc.; halogenated hydrocarbon groups such as chloromethyl, chloropropyl, and chlorocyclohexyl. Preferably it is an alkyl group, more preferably it is a methyl group.

The alkenyl group represented by R ² is not particularly limited, but is preferably an alkenyl group having 2 to 10 carbon atoms such as vinyl, allyl, and ethynyl, more preferably an alkenyl group having 2 to 6 carbon atoms, and More preferably, it is vinyl.

As a specific example of a branched organopolysiloxane, the one represented by the following formula etc. are mentioned, for example.

(上述式中，括弧內之矽氧烷單位之排列順序可為任意)。 (A)成分可單獨使用一種，亦可併用兩種以上。For component (A), organopolysiloxanes having a linear molecular structure can also be used. As a specific example of the linear organopolysiloxane, one represented by the following formula is exemplified.

(In the above formula, the order of the siloxane units in parentheses can be arbitrary). (A) A component may be used individually by 1 type, and may use 2 or more types together.

<Component (B)> The component (B) is represented by the following average composition formula (1), and is a waxy or solid three-dimensional network organopolysiloxane at 23°C. (B) The component is used to maintain the transparency of the hardened material and obtain reinforcement. It contains at least one of the _{alkenyl group bonded to the silicon atom and the SiO 3/2} unit or the SiO _{4/2 unit in the molecule.} Three-dimensional network of organopolysiloxane resin. Here, the so-called "waxy" means that the viscosity at 23°C is 10,000,000 mPa･s or more, especially 100,000,000 mPa･s or more, which is rubbery (raw rubber) that hardly shows self-flowing properties.

(式中，R¹ 及R² 與前述相同，a、b、c、d、e、f、g及h分別為滿足a≧0、b≧0、c≧0、d≧0、e≧0、f≧0、g≧0及h≧0之數，但係滿足b+c＞0，f+g+h＞0且a+b+c+d+e+f+ g+h=1之數)。

(In the formula, R ¹ and R ^{2 are the} same as the above, a, b, c, d, e, f, g, and h respectively satisfy a≧0, b≧0, c≧0, d≧0, e≧0 , F≧0, g≧0 and h≧0, but satisfying b+c>0, f+g+h>0 and a+b+c+d+e+f+g+h=1 ).

Examples of R ¹ are the same as those exemplified in the component (A), preferably an alkyl group having 1 to 8 carbon atoms, and more preferably a methyl group. Examples of R ² are the same as those exemplified in the component (A), preferably an alkenyl group having 2 to 10 carbon atoms, more preferably an alkenyl group having 2 to 6 carbon atoms, and still more preferably a vinyl group. Preferably, a is 0 to 0.65, b is 0.1 to 0.65, c is 0 to 0.65, d is 0 to 0.5, e is 0 to 0.5, f is 0 to 0.8, g is 0 to 0.8, and h is 0 to 0.6. number. Also, f+g+h is preferably 0.05 or more, more preferably a number of 0.1 to 0.9, and still more preferably a number of 0.2 to 0.6.

In the component (B), the content of the alkenyl group bonded to the silicon atom is preferably in the range of 0.01 to 1 mol per 100 g of the component (B), more preferably in the range of 0.1 to 0.6 mol. If the above content is in the range of 0.01 to 1 mol, the cross-linking reaction proceeds sufficiently to obtain a hardened product with higher hardness.

The component (B) preferably has R ² ₃ SiO _1/2 unit and SiO _4/2 unit (that is, b>0 and h>0). In this case, it is possible to impart adhesive strength to the cured product obtained from the composition. In addition, the branch structure of the component (B) composed of SiO _4/2 units and/or SiO _3/2 units is necessary, but it can also contain methyl vinyl siloxy units and dimethyl siloxy units. SiO _2/2 (SiO) unit, dimethyl vinyl siloxy unit, trimethyl siloxy unit, etc. SiO _1/2 unit. The content of SiO _4/2 unit and/or SiO _3/2 unit is preferably at least 5 mol% of all silicone units in the organopolysiloxane resin of component (B), more preferably 10 mol~ 95 mol%, particularly preferably 20-60 mol%.

The content of (B) component is 70 to 95 parts by mass, preferably 75 to 95 parts by mass, more preferably 80 to 90 parts by mass relative to 100 parts by mass of the total of (A) and (B) components. (B) When the blending amount of the component is less than 70 parts by mass, the adhesion may be poor and a hardened product with high hardness may not be obtained. When it exceeds 95 parts by mass, the viscosity of the composition becomes significantly higher, and the transfer becomes difficult. It becomes difficult to handle when used in bonding crystal materials.

(B)成分可單獨使用一種亦可併用兩種以上。As a specific example of (B) component, the following are mentioned, for example.

(B) A component may be used individually by 1 type, and may use 2 or more types together.

(式中，R¹ 與前述相同，i及j係滿足0.7≦i≦2.1、0.001≦j≦1.0且0.8≦i+j≦3.0之數)。<(C) Component> The (C) component functions as a crosslinking agent that crosslinks by the hydrosilylation reaction with the alkenyl group contained in the (A) component and (B) component. The component (C) is an organohydrogenpolysiloxane having at least two hydrogen atoms (ie, Si-H groups) bonded to silicon atoms in one molecule represented by the following average composition formula (2).

(In the formula, R ¹ is the same as above, and i and j satisfy the number of 0.7≦i≦2.1, 0.001≦j≦1.0, and 0.8≦i+j≦3.0).

Examples of R ¹ are the same as those exemplified in the component (A), preferably an alkyl group having 1 to 8 carbon atoms, and more preferably a methyl group. Furthermore, in the composition of the present invention, the ratio of the methyl group to the total number of all monovalent hydrocarbon groups bonded to the silicon atom other than the alkenyl group represented ^{by R 1 is preferably 80 mol% or more (that is, the aforementioned R 1} , 80 mol% or more are methyl groups), particularly preferably 90 mol% or more, due to deterioration of heat resistance, light resistance (ultraviolet resistance), and discoloration caused by stress such as heat and ultraviolet rays It is preferable because it has excellent resistance. The component (C) has at least two in one molecule, preferably 2 to 200, more preferably 3 to 100, and more preferably 4 to 50 hydrogen atoms (Si-H groups) bonded to silicon atoms.

The blending amount of (C) component is based on the viewpoint of cross-linking balance, relative to all the alkenyl groups in (A) and (B) that are bonded to silicon atoms, and the hydrogen atom of (C) component is bonded to silicon atoms The (Si-H group) number becomes 0.5 to 5.0 times, preferably 0.7 to 3.0 times. If the number of the aforementioned hydrogen atoms is less than 0.5 times the total number of the aforementioned alkenyl groups, crosslinking will not proceed sufficiently, and a cured product having excellent hardness will not be obtained. If the number of the aforementioned hydrogen atoms is more than 5.0 times the total number of the aforementioned alkenyl groups, the silicone cured product lacks flexibility and the silicone cured product becomes brittle.

(C) The viscosity of the component at 25°C is not particularly limited, but is preferably 100 mPa･s or less, and more preferably in the range of 5 to 100 mPa･s.

(C) The mass of the component after heating at 150°C under 1 atmosphere pressure for 30 minutes decreases, and it is preferably 1 mass% or less with respect to the mass before heating. If it is in this range, the contamination of the gold pad can be further reduced. (C) The molecular structure of the organohydrogen polysiloxane of the component can be any of linear, cyclic, branched, or three-dimensional network structure. The number of silicon atoms in one molecule is preferably 10 to 300 , More preferably 50~200. If so, a composition with less volatile matter during hardening and less contamination of the gold pad can be obtained.

(式中，R¹ 如前述，t為2~40，較佳為8~35之整數，u為6~8之整數)。The organohydrogen polysiloxane as the component (C) can be exemplified by 1,1,3,3-tetramethyldisiloxane, 1,3,5,7-tetramethylcyclotetrasiloxane, tri (Hydrogen dimethyl siloxy) methyl silane, tris (hydro dimethyl siloxy) phenyl silane, methyl hydrogen ring polysiloxane, methyl hydrogen siloxane, dimethyl siloxane ring -Like copolymer, both ends of trimethylsiloxy-terminated methylhydropolysiloxane, both ends of trimethylsiloxy-terminated dimethylsiloxane, methylhydrosiloxane copolymer, both ends Dimethylhydrosiloxy-terminated dimethylpolysiloxane, two-terminal dimethylhydrosiloxy-terminated methylhydropolysiloxane, two-terminal dimethylhydrosiloxy-terminated dimethylpolysiloxane Silicone, methylhydrosiloxane copolymer, trimethylsiloxy terminated methylhydrosiloxane at both ends, diphenylsiloxane copolymer, trimethylsiloxy terminated methyl at both ends Hydrogen siloxane, diphenyl siloxane, dimethyl siloxane copolymer, trimethyl siloxy terminated methyl hydrosiloxane at both ends, methyl phenyl siloxane, dimethyl Silicone copolymer, two-terminal dimethylhydrosiloxy-terminated methylhydrosiloxane, dimethylsiloxane, diphenylsiloxane copolymer, two-terminal dimethylhydrosiloxane-terminated methylhydrosiloxane End methylhydrosiloxane, dimethylsiloxane, methylphenylsiloxane copolymer, composed of (CH ₃ ) ₂ HSiO _1/2 unit, (CH ₃ ) ₃ SiO _1/2 unit and SiO _{4 /2} units, copolymers composed of (CH ₃ ) ₂ HSiO _1/2 units and SiO _4/2 units, copolymers composed of (CH ₃ ) ₂ HSiO _1/2 units, SiO _4/2 units, and (C ₆ H ₅ ) ₃ SiO _1/2 unit composed of copolymers, etc., and also exemplified by the following general formula (6) or (7).

(In the formula, R ^{1 is} as mentioned above, t is 2-40, preferably an integer of 8 to 35, and u is an integer of 6 to 8).

(式中，t如前述，Me為甲基)、 以下述式表示者等。As a specific example of the component (C), one represented by the following formula (8) is exemplified,

(In the formula, t is as described above, and Me is a methyl group), those represented by the following formula, and the like.

(上述式中，括弧內之矽氧烷單位之排列順序為任意)。

(In the above formula, the order of the siloxane units in parentheses is arbitrary).

(C) The organohydrogen polysiloxane of the component may be used alone or in combination of two or more.

(式中，R¹ 與前述相同，R³ 分別為相同或不同之含環氧基之基，R⁴ 分別相同或不同為不含烯基之取代或非取代之一價烴基，k及m分別為滿足k＞0、m≧0及k+m=1之數，n係滿足0≦n≦2之數)。<(D) component> The (D) component is an epoxy group-containing polysiloxane represented by the following formula (3).

(In the formula, R ¹ is the same as above, R ³ is the same or different epoxy-containing group, R ^{4 is the} same or different, is a substituted or unsubstituted monovalent hydrocarbon group without alkenyl, k and m are respectively In order to satisfy the number of k>0, m≧0 and k+m=1, n is a number satisfying 0≦n≦2).

Since the component (D) of the present invention is a _{polymer formed by repeating SiO 3/2} units, it can provide a composition with fewer low-molecular components, improved adhesion, and no gold pad contamination.

(式中，s為1~6之整數，虛線表示鍵結鍵)。 R¹ 舉例為與(A)成分中例示者相同者，較佳為碳原子數1~8之烷基，更佳為甲基。The epoxy group-containing group represented by R ³ is exemplified by an alicyclic epoxy group or a glycidyl group bonded to a silicon atom via a carbon atom, and preferably has a glycidyl group. More preferred are groups represented by the following formula (5) such as γ-glycidoxypropyl, and β-(3,4-epoxycyclohexyl)ethyl.

(In the formula, s is an integer from 1 to 6, and the dashed line represents the bonding bond). Examples of R ¹ are the same as those exemplified in the component (A), preferably an alkyl group having 1 to 8 carbon atoms, and more preferably a methyl group.

The substituted or unsubstituted monovalent hydrocarbon group not containing an alkenyl group represented by R ⁴ is not particularly limited if it does not have an alkenyl group, but it is preferably one of substituted or unsubstituted carbon atoms having 1 to 8 Valence hydrocarbon group. Examples of monovalent hydrocarbon groups include alkyl groups such as methyl, ethyl, propyl, and butyl, cycloalkyl groups such as cyclohexyl and cyclopentyl, aryl groups such as phenyl, tolyl and xylyl, and benzyl Alkyl groups such as chloromethyl, phenethyl groups, and halogenated hydrocarbon groups such as chloromethyl, chloropropyl, and chlorocyclohexyl groups. Preferred are alkyl groups, and particularly preferred are methyl and ethyl groups.

(D) The mass of the component after heating at 150°C for 30 minutes under 1 atmosphere is reduced, and it is preferably 5% by mass or less with respect to the mass before heating. If it is in this range, the contamination of the gold pad can be further reduced. (D) The component is preferably liquid, and if it is in the range of molecular weight 500 to 10,000, it is preferable from the viewpoint of workability and prevention of contamination of the gold pad. In formula (3), k and m are preferably numbers satisfying 0<k≦0.9, 0<m≦0.9, and k+m=1. If the component (D) is in this range, the compatibility of the components (A), (B), and (C) is excellent, and the obtained hardened product has excellent adhesiveness and grain shear strength. From the viewpoint of the preservation stability of the composition and the prevention of contamination of the gold pad, n is preferably a number of 0 to 1, more preferably a number of 0 to 0.1, and even more preferably 0.

The amount of (D) component is 1 to 25 parts by mass, preferably 3 to 10 parts by mass relative to 100 parts by mass of the total of (A), (B), and (C) components. If the amount does not reach the lower limit, there are cases where the desired grain shear strength cannot be obtained. In addition, when the amount exceeds the upper limit, components in the composition may separate, and the strength of the resulting hardened product may decrease.

＜(E) Ingredient＞ The platinum group metal catalyst of the component (E) is a component used to carry out and promote the hydrosilylation reaction of the aforementioned components (A) to (C).

The platinum group metal catalyst is not particularly limited, and examples thereof include platinum group metals such as platinum, palladium, and rhodium; chloroplatinic acid, alcohol-modified chloroplatinic acid, chloroplatinic acid and olefins, vinyl silica Platinum compounds such as coordination compounds of alkanes or acetylene compounds; platinum group metal compounds such as tetrakis(triphenylphosphine)palladium, chlorotris(triphenylphosphine)rhodium, etc., but due to the compatibility with components (A)~(C) It has good solubility and almost no chlorine impurities, so it is preferably chloroplatinic acid modified by silicone. (E) A component may be used individually by 1 type, and may use 2 or more types together.

The compounding amount of (E) component is 1 to 500 ppm, preferably 3 to 100 ppm, and more preferably 5 to 40 ppm in terms of the mass of platinum group metal elements relative to the total mass of (A) to (D) components. (E) When the blending amount of component does not reach the lower limit, the obtained polysiloxane composition for crystal bonding is not sufficiently hardened. On the other hand, even if the blending exceeds the upper limit of the above range, the obtained polysiloxane composition for crystal bonding cannot be increased. The hardening speed of things.

<(F) Component> The polysiloxane composition for crystal bonding of the present invention may contain fumed silica as the (F) component. The component (F) is a component for stably coating the polysiloxane composition for crystal bonding of the present invention and imparting appropriate thixotropy. From the viewpoint of thixotropy and workability, the BET specific surface area of the component (F) is preferably in ^{the range of 100 to 400 m 2} /g.

From the viewpoint of thixotropy and workability, the blending amount of the (F) component is preferably added in the range of 3 to 10 parts with respect to 100 parts by mass of the (A) to (E) components. As a specific example of the component (F), REOLOSIL DM-30 (manufactured by TOKUYAMA (stock), BET specific surface area 300 m ² /g), etc. are exemplified.

＜Other ingredients＞ In addition to the above-mentioned (A) to (F) components, the composition of the present invention may also contain other components exemplified below. (Reaction inhibitor) In the silicone composition for crystal bonding of the present invention, a conventional reaction inhibitor (reaction control agent) having a curing inhibitory effect on the addition reaction catalyst of the component (D) can be used as needed. Examples of the reaction inhibitor include phosphorus-containing compounds such as triphenylphosphine; nitrogen-containing compounds such as tributylamine, tetramethylethylenediamine, benzotriazole, etc.; sulfur-containing compounds; acetylene-based compounds; hydrogen peroxide compounds ; Maleic acid derivatives and so on.

The degree of the hardening inhibitory effect of the reaction inhibitor varies greatly with the chemical structure of the reaction inhibitor. Therefore, the compounding amount of the reaction inhibitor is preferably adjusted to the most appropriate amount for each reaction inhibitor used. Usually, it is preferable that it is 0.001-5 mass parts with respect to the total of 100 mass parts of (A) component, (B) component, (C) component, and (D) component.

(Filler) In addition to the fuming silica of component (F), the silicone composition for crystal bonding of the present invention can also be filled with inorganic fillers such as crystalline silica, hollow filler, silsesquioxane, etc.; and The filler is used for surface hydrophobization of organosilicon compounds such as organoalkoxysilane compounds, organochlorosilane compounds, organosilazane compounds, low molecular weight silicone compounds, etc.; silicone rubber powder; polysilicone Silicone resin powder, etc. As this ingredient, based on workability, a filler that can impart thixotropy is particularly preferably used. These other components may be used individually by 1 type, and may use 2 or more types together.

In addition, it is preferable that 80 mol% or more ^{of all R 1} in the polysiloxane composition for crystal bonding of the present invention is a methyl group. In addition, in order to improve the workability of die bonding (transfer method), the viscosity of the polysiloxane composition for die bonding of the present invention is preferably 5-100 Pa･s, more preferably 20-50 Pa･ at 25°C s.

[Hardened material] Furthermore, the present invention provides a cured product (polysilicon cured product) of a polysilicon composition for crystal bonding. The curing of the polysilicone composition for crystal bonding of the present invention can be carried out under conventional conditions. As an example, it can be cured at 100-180°C for 10 minutes to 5 hours.

The cured product of the polysilicon oxide composition for die bonding of the present invention has high adhesion to substrates, LED chips, etc., and is particularly useful as a die bonding material for die bonding of LED devices and the like. As described above, the silicone cured product according to the present invention can be an adhesive with high adhesion to substrates, LED chips, and the like.

[Optical Semiconductor Device] Furthermore, the present invention provides an optical semiconductor device in which an optical semiconductor element is bonded with the aforementioned hardened material. As an example of a method of using the polysilicon oxide composition for die bonding of the present invention to bond an optical semiconductor device, for example, filling the polysilicon oxide composition for die bonding of the present invention in a syringe, and using a glue applicator for packaging After coating the substrate in a dry state to a thickness of 1-100 μm, arrange an optical semiconductor element (such as a light-emitting diode) on the coated composition to harden the composition, thereby hardening the light A method of bonding semiconductor components to a substrate. Alternatively, the composition is placed in a rubber roller tray, and the substrate is coated with a thickness of 1~100μm in a dry state by pressing while pressing, and then on the coated composition A method of disposing the optical semiconductor element to harden the composition, thereby bonding the optical semiconductor element to the substrate. The curing conditions of the composition may be as described above. In this way, it is possible to become an optical semiconductor device with high reliability, and the optical semiconductor device is bonded with the polysilicon cured material of the present invention. [Example]

The following examples and comparative examples are used to specifically illustrate the present invention, but the present invention is not limited to these. In addition, the molecular weight is the weight average molecular weight in terms of standard polystyrene in gel permeation chromatography (GPC). The viscosity at 25°C is measured by a rotary viscometer. The volatile matter is the mass reduction (mass%) when heated at 150°C for 30 minutes under 1 atmosphere. In addition, the meaning of the abbreviation of each silicone unit is as follows. M: (CH ₃ ) ₃ SiO _1/2 M ^Vi : (CH ₂ =CH)(CH ₃ ) ₂ SiO _1/2 M ^Vi3 : (CH ₂ =CH) ₃ SiO _1/2 D: (CH ₃ ) ₂ SiO _2/2 D ^H : H(CH ₃ )SiO _2/2 T: (CH ₃ )SiO _3/2

T ¹ :

T ² :

T ³ :

T ⁴ :

Q：SiO_4/2 T ⁵ :

Q: SiO _4/2

[Synthesis Example 1] A 3,000 mL 4-necked flask equipped with a stirring device, a cooling tube, a dropping funnel, and a thermometer was charged with [(CH ₃ O) ₃ SiO _1/2 ] ₂ [(CH ₃ O) ₂ SiO] ₂ represents 352.5g of organopolysiloxane, 45.6g of hexavinyldisiloxane, 182.3g of hexamethyldisiloxane, 58g of isopropanol, and 6.7g of methanesulfonic acid is dropped while stirring. Subsequently, 90 g of water was dropped, and the mixture was mixed at 65°C for 2 hours to perform the reaction. 700 g of xylene and 10.9 g of a 50% potassium hydroxide aqueous solution were added thereto, and the reaction was carried out at 120° C. for 5 hours while distilling off low-boiling components at elevated temperature. Add 3.5 g of methanesulfonic acid as an additive, and perform neutralization treatment at 120°C for 2 hours. After cooling, filter to obtain a ^{three-dimensional network organopolysiloxane with a composition ratio of M Vi3} _0.07 M _0.4 Q _0.53 (B-1: molecular weight 3,350, solid at 23°C, relative to the amount of vinyl in the solid content 0.287 mol/100g).

[Synthesis Example 2] A 1,000 mL 4-necked flask equipped with a stirring device, a cooling tube, a dropping funnel and a thermometer was charged with 234 g of 3-glycidoxypropyltrimethoxysilane, 136 g of methyltrimethoxysilane, and methanol 37.8 g, a mixed solution of 29 g of 0.04N hydrochloric acid and 70.3 g of methanol was dropped while stirring. After reacting at 25°C for 3 hours while stirring, a 10% sodium acetate/methanol solution was dropped to neutralize, and stirring was performed at 65°C for 2 hours. After cooling and filtering, add 500g of methanol/water (mass ratio 50:50) mixed solution, mix for 20 minutes, let stand for 30 minutes, and repeat the washing operation of separating and removing the methanol solvent layer 3 times to remove low molecules Then, it was concentrated under reduced pressure at 100°C for 1 hour to remove remaining methanol. After cooling to 25°C, filtration was performed to obtain epoxy-containing siloxane (D-1: molecular weight 2,780, viscosity 313 mPa･s) ^{with a structural unit ratio of T 1} _0.49 T _0.51. The volatile content is 1.7% by mass.

[Synthesis Example 3] A 1,000 mL 4-necked flask equipped with a stirring device, a cooling tube, a dropping funnel, and a thermometer was charged with 304 g of 8-glycidoxyoctyl trimethoxysilane, 136 g of methyl trimethoxysilane, and methanol 37.8 g, a mixed solution of 29 g of 0.04N hydrochloric acid and 70.3 g of methanol was dropped while stirring. After reacting at 25°C for 3 hours while stirring, a 10% sodium acetate/methanol solution was dropped to neutralize, and stirring was performed at 65°C for 2 hours. After cooling to 25°C and filtering, 500 g of a methanol/water (mass ratio 50:50) mixed solution was added, mixed for 20 minutes, allowed to stand for 30 minutes, and the washing operation of separating and removing the methanol solvent layer was repeated 3 times, and The low molecular weight was removed, and further concentrated under reduced pressure at 100°C for 1 hour to remove remaining methanol. After cooling to 25°C, filtration was performed to obtain epoxy-containing siloxane (D-2: molecular weight 2,570, viscosity 138mPa･s) ^{with a structural unit ratio of T 2} _0.47 T _0.53. The volatile content is 1.5% by mass.

[Synthesis Example 4] A 1,000 mL 4-necked flask equipped with a stirring device, a cooling tube, a dropping funnel, and a thermometer was charged with 246 g of 2-(3,4-epoxycyclohexyl)trimethoxysilane and methyltrimethoxy 136 g of silyl silane, 37.8 g of methanol, and a mixed solution of 29 g of 0.04N hydrochloric acid and 70.3 g of methanol was dropped while stirring. After reacting at 25°C for 3 hours while stirring, a 10% sodium acetate/methanol solution was dropped to neutralize, and stirring was performed at 65°C for 2 hours. After cooling to 25°C and filtering, 500 g of a methanol/water (mass ratio 50:50) mixture was added, mixed for 20 minutes, allowed to stand for 30 minutes, and the washing operation of separating and removing the methanol solvent layer was repeated 3 times. The low molecular weight was removed, and further concentrated under reduced pressure at 100°C for 1 hour to remove remaining methanol. After cooling to 25°C, filtration was performed to obtain epoxy-containing siloxane (D-3: molecular weight 1890, viscosity 137 mPa･s) ^{with a structural unit ratio of T 3} _0.57 T _0.43. The volatile matter (150°C for 30 minutes) was 4.7% by mass.

[Comparative Synthesis Example 1] A 1,000 mL 4-necked flask equipped with a stirring device, a cooling tube, a dropping funnel, and a thermometer was charged with 248 g of 3-methacryloxypropyltrimethoxysilane and methyltrimethoxysilane 136 g, 37.8 g of methanol, and a mixed solution of 29 g of 0.04N hydrochloric acid and 70.3 g of methanol was dropped while stirring. After reacting at 25°C for 3 hours while stirring, a 10% sodium acetate/methanol solution was dropped to neutralize, and stirring was performed at 65°C for 2 hours. After cooling to 25°C and filtering, 500 g of a methanol/water (mass ratio 50:50) mixture was added, mixed for 20 minutes, allowed to stand for 30 minutes, and the washing operation of separating and removing the methanol solvent layer was repeated 3 times. The low molecular weight was removed, and further concentrated under reduced pressure at 100°C for 1 hour to remove remaining methanol. After cooling to 25°C, filtration was performed to obtain ^{an organopolysiloxane having a unit ratio of T 4} _0.52 T _0.48 (D-4: molecular weight 2,900, viscosity 261 mPa･s). The volatile content is 2.7% by mass.

[Comparative Synthesis Example 2] A 1,000 mL 4-necked flask equipped with a stirring device, a cooling tube, a dropping funnel and a thermometer was charged with 248 g of 3-propenoxypropyltrimethoxysilane, 136g of methyltrimethoxysilane, With 37.8 g of methanol, a mixed solution of 29 g of 0.04N hydrochloric acid and 70.3 g of methanol was dropped while stirring. After reacting at 25°C for 3 hours while stirring, a 10% sodium acetate/methanol solution was dropped to neutralize, and stirring was performed at 65°C for 2 hours. After cooling to 25°C and filtering, 500 g of a methanol/water (mass ratio 50:50) mixture was added, mixed for 20 minutes, allowed to stand for 30 minutes, and the washing operation of separating and removing the methanol solvent layer was repeated 3 times. The low molecular weight was removed, and further concentrated under reduced pressure at 100°C for 1 hour to remove remaining methanol. After cooling to 25°C, filtration was performed to obtain ^{an organopolysiloxane with a unit ratio of T 5} _0.49 T _0.51 (D-5: molecular weight 3,350, viscosity 387 mPa･s). The volatile content is 0.9% by mass.

[Synthesis Example 5] The reaction product of hexachloroplatinic acid and 1,3-divinyltetramethyldisiloxane is a linear chain represented ^{by M Vi} ₂ D _{40 so that the platinum content becomes 0.004% by mass} Dimethyl polysiloxane (viscosity 60 mPa･s) is diluted to prepare platinum catalyst.

[Examples 1 to 4, Comparative Examples 1 to 7] The following components were mixed in the blending amounts shown in Table 1 to prepare a silicone resin composition for crystal bonding. In addition, the numerical value of each component in Table 1 represents parts by mass. The value of [Si-H]/[Si-Vi] indicates that the hydrogen atom (Si-H) in the component (C) bonded to the silicon atom is relative to the component (A) and the component (B) bonded to the silicon atom The ratio of the total number of all alkenyl groups (molar ratio).

(A) Component: (A-1) ^{Organopolysiloxane expressed by the component ratio M Vi} _0.47 T _0.53 (Viscosity at 25°C 17mPa･s) (A-2) The average structure is M ^Vi ₂ D ₁₅ The linear dimethylpolysiloxane expressed (viscosity at 25℃ is 8.8mPa･s) (A-3) has an average structure of M ^Vi ₂ D ₂₀₄ expressed dimethylpolysiloxane (at 25℃ The viscosity is 600mPa･s)

(B) Component: (B-1) The three-dimensional network organopolysiloxane (B-2) obtained in Synthesis Example 1 has an average structure of M ^Vi _1.2 M _7.4 Q ₁₀ represents the amount of vinyl that is solid at 23°C 0.085mol/100g three-dimensional network organopolysiloxane

(C) Component: _{Organohydrogen polysiloxane represented by an average structure of M 2} D 14.5 D ^H ₃₈ (the volatile content is 0.2% by mass)

(D) Ingredients: (D-1) Organopolysiloxane obtained in Synthesis Example 2 (The volatile content is 1.7% by mass) (D-2) Organopolysiloxane obtained in Synthesis Example 3 (the volatile content is 1.5% by mass) (D-3) Organopolysiloxane obtained in Synthesis Example 4 (The volatile content is 4.7% by mass) (D-4) Organopolysiloxane obtained in Comparative Synthesis Example 1 (the volatile content is 2.7% by mass) (D-5) The organopolysiloxane obtained in Comparative Synthesis Example 2 (the volatile content is 0.9% by mass) (D-6)3-Glycidoxypropyltrimethoxysilane (97% by mass volatile)

(D) The volatile component of the component is the result of applying 1.5g of each component (D) on a Φ60mm aluminum pan successively, heating it in an open system at 150°C for 30 minutes, and calculating the mass reduction after heating.

(E) Component: The platinum catalyst obtained in Synthesis Example 5 (F) Component: Fuming silica [REOLOSIL DM30 (manufactured by TOKUYAMA, BET specific surface area 300m ² /g)] (G) Reaction inhibitor: 1-ethynyl ring Hexanol

The following evaluations were performed on the polysiloxane compositions for crystal bonding obtained in Examples 1 to 4 and Comparative Examples 1 to 7. The results are shown in Table 1. [hardness] The aforementioned composition was poured into a mold so as to be 2 mm thick, and cured under the conditions of 150° C.×4 hours. D type hardness basis of hardened material Measured in JIS K 6253-3:2012.

[Grain Shear Strength] The aforementioned composition uses a die bonder (manufactured by ASM, AD-830), and the silver-plated electrode part of the SMD5730 package (manufactured by I-CHIUN PRECSION INDUSTRY CO., resin part: polyxylylenedimethamide) is processed by pressing Quantitative transfer. Wire drawing occurred during punching and the resin could not be transferred was marked as ×, and the case where there was no problem but could be transferred was marked as ○. Furthermore, an optical semiconductor element (manufactured by SemiLEDs, EV-B35A, 35mil) was mounted on it. The manufactured package was heated in an oven at 150°C for 4 hours to harden the composition, and then the grain shear strength was measured using a bonding tester (manufactured by Dage Corporation, 4000 series).

[Gold pad contamination] A PKG equipped with an optical semiconductor element (EV-B35A, 35mil, manufactured by SemiLEDs) is installed on a Φ105mm aluminum plate, and 2g of resin is coated around the PKG. Then, after curing at 150°C for 4 hours, observe the gold pads of the semiconductor device under a microscope. The adhesion of silicone components on the gold pads is recorded as ×, and the absence of adhesion is recorded as ○.

As shown in Table 1, all Examples 1 to 4 had no defects at the time of punching, and were the result of the hardness of the hardened product, the excellent grain shear strength and no gold pad contamination, and it can be seen that they were excellent as a sticky material. In addition, the results of the gold pad contamination test of Example 1 are shown in FIG. 1.

On the other hand, Comparative Example 1 does not contain the (D) component, and the crystal grain strength becomes insufficient. In Comparative Example 2, since the (D) component does not contain an epoxy group, the result is that the grain shear strength is inferior. The comparative example 4 series (A) component has a high viscosity and is a sticky material which cannot be punched and has poor workability, and the comparative example 5 series (D) has a low component and low grain shear strength. In Comparative Example 6, because the component (D) was too much, the hardening of the hardened product was sufficient, but the composition was separated, and when it was used as a viscous material, it had no storage properties and resulted in poor reliability. In Comparative Example 7, although the crystal grain shear strength was slightly improved by the epoxy-containing silane coupling agent, as shown in FIG. 2, contamination of the gold pad occurred, resulting in poor reliability.

As described above, the polysiloxane composition for die bonding of the present invention can impart a cured polysiloxane with excellent hardness and grain shear strength, and can effectively inhibit the contamination of gold pads during hardening. It can be used as an optical semiconductor device, etc. The die-bonding materials used in die-bonding are particularly useful. In particular, due to this advantage, it is difficult for the wafer to peel off or fail to be bonded in the wire bonding step after the die bonding step. Therefore, the optical semiconductor device in which the optical semiconductor element is bonded by the polysiloxy hardened material is reliable. Improve the productivity of the device. Therefore, the polysilicon oxide composition for die bonding and its cured product of the present invention have high utility value in the technical field of optical semiconductor devices.

In addition, the present invention is not limited to the above-mentioned embodiment. The above-mentioned embodiment is an example, and any one having substantially the same structure as the technical idea described in the scope of the patent application of the present invention and exerting the same effect is included in the technical scope of the present invention.

[Figure 1] is a photograph of the appearance of the gold pad contamination test of Example 1. [Figure 2] is a photograph of the appearance of the gold pad contamination test of Comparative Example 7.

Claims (10)

A polysiloxane composition for crystal bonding, which is characterized by containing the following components (A) ~ (E), (A) contains 2 or more alkenyl groups per molecule, and has a viscosity of 100mPa･s at 25°C The following organopolysiloxanes, (B) are represented by the following formula (1), which are waxy or solid three-dimensional network organopolysiloxanes at 23°C: relative to the ratio of (A) component and (B) component A total of 100 parts by mass, 70 to 95 parts by mass,

(In the formula, R ¹ are the same or different, substituted or unsubstituted monovalent hydrocarbon group without alkenyl, R ² are the same or different alkenyl, a, b, c, d, e, f, g And h are the numbers satisfying a≧0, b≧0, c≧0, d≧0, e≧0, f≧0, g≧0, and h≧0, but satisfying b+c>0, f+ g+h>0 and a+b+c+d+e+f+g+h=1) (C) is represented by the following average composition formula (2), and there are at least 2 bonds in one molecule to silicon The organohydrogen polysiloxane of the hydrogen atom of the atom: relative to the total number of the alkenyl groups in the (A) component and the (B) component bonded to the silicon atom, the (C) component is bonded to the silicon atom The number of hydrogen atoms becomes 0.5~5.0 times the amount,

(In the formula, R ¹ is the same as the above, i and j are the numbers satisfying 0.7≦i≦2.1, 0.001≦j≦1.0, and 0.8≦i+j≦3.0) (D) Containing ring represented by the following formula (3) Polysiloxane of oxy group: 1-25 parts by mass relative to 100 parts by mass of the total of (A) component, (B) component and (C) component,

(In the formula, R ¹ is the same as above, R ³ is the same or different epoxy-containing group, R ^{4 is the} same or different, is a substituted or unsubstituted monovalent hydrocarbon group without alkenyl, k and m are respectively In order to satisfy the number of k>0, m≧0 and k+m=1, the n system satisfies the number of 0≦n≦2), (E) platinum group metal catalyst: relative to (A) component, (B) The total mass of components, (C) components, and (D) components is 1 to 500 ppm in terms of the mass of platinum metal elements. Such as the polysiloxane composition for crystal bonding of claim 1, wherein the aforementioned component (A) is an organopolysiloxane represented by the following formula (4),

(In the formula, R ¹ and R ^{2 are the} same as above, o, p, q, r are the numbers satisfying q≧0, r≧0, o≧0, p≧0, but satisfying q+r>0, r+o>0, o+p>0 and o+p+q+r=1). For example, the polysilicon oxide composition for crystal bonding of claim 1, wherein in the aforementioned formula (1), b>0 and h>0. The polysiloxane composition for crystal bonding according to any one of claims 1 to 3, wherein the aforementioned component (C) has a mass reduction of 1% by mass or less when heated at 150°C for 30 minutes under 1 atmosphere. The polysiloxane composition for crystal bonding according to any one of claims 1 to 3, wherein the aforementioned component (D) has a mass reduction of 5 mass% or less when heated at 150°C for 30 minutes under 1 atmosphere. The polysiloxane composition for crystal bonding according to any one of claims 1 to 3, wherein in the aforementioned component (D), R ³ is a base represented by the following formula (5),

(In the formula, s is an integer from 1 to 6, and the dashed line represents the bonding bond). The polysiloxane composition for crystal bonding according to any one of claims 1 to 3, wherein more than 80 mol% ^{of all R 1 in the aforementioned composition are methyl groups.} The polysilicon oxide composition for crystal bonding according to any one of claims 1 to 3, which further contains (F) ^{fumed silica with a BET specific surface area of 100-400 m 2} /g. A cured polysilicone characterized by a cured polysilicone composition for crystal bonding according to any one of claims 1 to 8. An optical semiconductor device characterized in that an optical semiconductor element is bonded with a polysilicon cured material as in Claim 9.

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