WO2015005138A1 - Method for transporting sealing resin composition and packaging - Google Patents
Method for transporting sealing resin composition and packaging Download PDFInfo
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- WO2015005138A1 WO2015005138A1 PCT/JP2014/067124 JP2014067124W WO2015005138A1 WO 2015005138 A1 WO2015005138 A1 WO 2015005138A1 JP 2014067124 W JP2014067124 W JP 2014067124W WO 2015005138 A1 WO2015005138 A1 WO 2015005138A1
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- resin composition
- packaging material
- sealing resin
- sealing
- temperature
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
- H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
- H01L21/565—Moulds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/31—Structure, shape, material or disposition of the layer connectors after the connecting process
- H01L2224/32—Structure, shape, material or disposition of the layer connectors after the connecting process of an individual layer connector
- H01L2224/321—Disposition
- H01L2224/32151—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
- H01L2224/32221—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
- H01L2224/32225—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being non-metallic, e.g. insulating substrate with or without metallisation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/42—Wire connectors; Manufacturing methods related thereto
- H01L2224/44—Structure, shape, material or disposition of the wire connectors prior to the connecting process
- H01L2224/45—Structure, shape, material or disposition of the wire connectors prior to the connecting process of an individual wire connector
- H01L2224/45001—Core members of the connector
- H01L2224/45099—Material
- H01L2224/451—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron (B), silicon (Si), germanium (Ge), arsenic (As), antimony (Sb), tellurium (Te) and polonium (Po), and alloys thereof
- H01L2224/45138—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron (B), silicon (Si), germanium (Ge), arsenic (As), antimony (Sb), tellurium (Te) and polonium (Po), and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
- H01L2224/45144—Gold (Au) as principal constituent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/42—Wire connectors; Manufacturing methods related thereto
- H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
- H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
- H01L2224/4805—Shape
- H01L2224/4809—Loop shape
- H01L2224/48091—Arched
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/42—Wire connectors; Manufacturing methods related thereto
- H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
- H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
- H01L2224/481—Disposition
- H01L2224/48151—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
- H01L2224/48221—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
- H01L2224/48225—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being non-metallic, e.g. insulating substrate with or without metallisation
- H01L2224/48227—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being non-metallic, e.g. insulating substrate with or without metallisation connecting the wire to a bond pad of the item
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/73—Means for bonding being of different types provided for in two or more of groups H01L2224/10, H01L2224/18, H01L2224/26, H01L2224/34, H01L2224/42, H01L2224/50, H01L2224/63, H01L2224/71
- H01L2224/732—Location after the connecting process
- H01L2224/73251—Location after the connecting process on different surfaces
- H01L2224/73265—Layer and wire connectors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/31—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape
- H01L23/3107—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape the device being completely enclosed
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/15—Details of package parts other than the semiconductor or other solid state devices to be connected
- H01L2924/151—Die mounting substrate
- H01L2924/153—Connection portion
- H01L2924/1531—Connection portion the connection portion being formed only on the surface of the substrate opposite to the die mounting surface
- H01L2924/15311—Connection portion the connection portion being formed only on the surface of the substrate opposite to the die mounting surface being a ball array, e.g. BGA
Definitions
- the present invention relates to a method for transporting a sealing resin composition and a package.
- Patent Document 1 discloses an invention relating to a packaging method for a semiconductor sealing epoxy resin molding material used for sealing a semiconductor element.
- a desiccant and the epoxy resin molding material for semiconductor sealing are put in the same bag and sealed.
- the present inventor provides a granular sealing resin composition used for sealing electronic components such as semiconductor elements, transistors, thyristors, diodes, solid-state imaging elements, capacitors, resistors, and LEDs, as follows. I found a problem.
- the sealing resin composition is accommodated in an inner packaging material such as a bag
- one or more inner packaging materials are accommodated in one outer packaging material such as a metal can or cardboard, and in this state It was stored and transported. And at the time of use, these packaging materials were opened, the sealing resin composition was taken out from the packaging materials, and the taken-out sealing resin composition was used.
- some of the encapsulating resin compositions solidify into a lump before being taken out from the packaging material for use after being contained in the packaging material. In some cases, it may be in a state where it is likely to become a lump (that is, a state where it becomes a lump in the transfer process described later).
- a semiconductor element is compression-molded
- such a lump is supplied to a predetermined place of a molding machine with a granular sealing resin composition taken out from a packaging material, transferred to a feeder or the like, and supplied with a resin material from the feeder.
- troubles occurred in the process of transferring to the container and weighing, and hindered smooth automatic molding.
- the wire may be deformed or unfilled.
- This invention makes it a subject to suppress the caking of some sealing resin compositions which may generate
- the granular sealing resin composition is contained in a packaging material, and the granular sealing resin composition is transported in a state of 10 ° C or less,
- the bulk density of the sealing resin composition is M (g / cc)
- M ⁇ L ⁇ 25 is satisfied,
- the packaging material containing the sealing resin composition was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours, and then taken out from the packaging material.
- the encapsulating resin composition is provided with a transport method in which the difference angle is 10 degrees or more.
- the granular sealing resin composition is contained in a packaging material, and the granular sealing resin composition is transported in a state of 10 ° C or less,
- the bulk density of the sealing resin composition is M (g / cc)
- M ⁇ L ⁇ 25 is satisfied,
- the packaging material containing the sealing resin composition was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours, and then taken out from the packaging material.
- the encapsulating resin composition is provided with a transport method in which the content of a sieve pass product having an opening of 2 mm is 90% by weight or more.
- Packaging materials A granular sealing resin composition housed in the packaging material; Have The packaging material containing the sealing resin composition was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours, and then taken out from the packaging material.
- the sealing resin composition is provided with a package having a difference angle of 10 degrees or more.
- Packaging materials A granular sealing resin composition housed in the packaging material; Have The packaging material containing the sealing resin composition was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours, and then taken out from the packaging material.
- the encapsulating resin composition provides a package in which the content of a sieve pass product having an opening of 2 mm is 90% by weight or more.
- the granular encapsulating resin composition contained in the packaging material (hereinafter sometimes simply referred to as “encapsulating resin composition”) is then transported to various places, but at a temperature of 10 ° C. or lower. It may be transported in a state where it is stored in a space kept at 10 ° C. or lower. And after conveying to a predetermined place, a sealing resin composition is returned to room temperature and used in the said state. In addition, after being transported to a predetermined place, it may be stored in a state of 10 ° C. or lower until it is used.
- the present inventor has fixed the sealing resin compositions between the sealing resin compositions by such a change in environment, that is, a change in environment in which the sample is left at a temperature of 10 ° C. or lower for a predetermined time and then returned to room temperature and left for a predetermined time. It has been found that ligation can be promoted. And it discovered newly that the problem of the consolidation of sealing resin composition can be reduced by controlling so that the sealing resin composition after the above environmental changes may be in an appropriate state.
- the transportation method of the present embodiment is a transportation method of a granular sealing resin composition that is contained in a packaging material and transported in a state of 10 ° C. or less, and includes the following (Condition 1) and (Condition 2) ), The sealing resin composition contained in the packaging material is transported.
- the present inventors transport the granular sealing resin composition accommodated in the packaging material under at least one of the following (Condition 1) and (Condition 2), the sealing resin compositions are fixed to each other. It was confirmed that the problem of culling could be reduced.
- the packaging material containing the sealing resin composition is allowed to stand for 24 hours at a temperature of 4 ° C. and a relative humidity of 35%, and then left for 24 hours at a temperature of 23 ° C. and a relative humidity of 50%.
- the encapsulating resin composition has a condition that the difference angle is 10 degrees or more. It should be noted that the condition that the difference angle is 11 degrees or more is preferable, and the condition that the difference angle is 12 degrees or more is more preferable. When the difference angle satisfies these conditions, reduction of caking troubles when the sealing resin composition is transported and weighed in the molding machine and suppression of wire deformation due to unevenness of the sealing resin composition on the mold This is preferable.
- the difference angle is the difference between the angle of repose and the collapse angle.
- a powder tester manufactured by Hosokawa Micron Co., Ltd.
- the like can be used as an apparatus for measuring the repose angle and the collapse angle.
- the packaging material containing the sealing resin composition is allowed to stand for 24 hours at a temperature of 4 ° C. and a relative humidity of 35%, and then left for 24 hours at a temperature of 23 ° C. and a relative humidity of 50%.
- the sealing resin composition thus prepared contains 90% by weight or more of a sieve pass product having an opening of 2 mm.
- the conditions which contain 95 weight% or more of sieve pass goods with an opening of 2 mm are more preferable.
- the sealing resin composition is excellent in reducing caking trouble when transporting and weighing in the molding machine and suppressing wire deformation due to unevenness of the sealing resin composition on the mold. Can be.
- a treatment in which the packaging material containing the sealing resin composition is allowed to stand at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours It is referred to as “room temperature return processing”.
- the present inventor believes that, when a normal temperature returning treatment is performed in a state where the granular sealing resin compositions are pressed against each other with a predetermined force or more, consolidation of the sealing resin compositions is promoted. It was. Then, at least one of the above conditions 1 and 2 is realized by controlling the force with which the encapsulating resin compositions are pressed against each other when the room temperature return treatment is performed so as to be equal to or less than a predetermined value (less than). It is possible to improve the suppression of wire deformation due to the reduction of caking trouble when the encapsulating resin composition is transported and measured in the molding machine and the unevenness of the encapsulating resin composition on the mold. I found out that I can do it.
- the force resulting from the weight of the sealing resin composition accommodated on the upper side is applied to the sealing resin composition accommodated on the lower side in the packaging material.
- the sealing resin composition positioned on the lower side in the packaging material includes: The force resulting from the weight of the sealing resin composition located on the upper side in the packaging material is applied.
- the sealing resin composition accommodated in the inner packaging material located on the lower side is positioned on the upper side. The force resulting from the weight of the sealing resin composition accommodated in the inner packaging material is applied.
- a means for controlling the force applied to the sealing resin composition (hereinafter referred to as “self-gravity”) was examined. That is, a means for appropriately controlling the maximum value of the self-gravity applied to the sealing resin composition, specifically, the maximum value of the self-gravity applied to the sealing resin composition positioned on the lower side was examined. And it discovered that at least one of the said conditions 1 and conditions 2 was realizable by controlling self-gravity appropriately.
- FIG. 1 shows an example of a schematic cross-sectional view of a granular sealing resin composition contained in a packaging material.
- the inner packaging material 20 is accommodated in the outer packaging material 10.
- M (g / cc) the bulk density of the sealing resin composition 30
- L (cm) the height of the deposit by the sealing resin composition 30 in the state accommodated in the packaging material.
- the present inventor has confirmed that when the sealing resin composition 30 described below is packaged so as to satisfy the condition, at least one of the above (condition 1) and (condition 2) is satisfied. .
- the difference angle after the room temperature return treatment becomes a preferable angle listed above.
- the content of the sieve pass product having an opening of 2 mm satisfies the above-mentioned preferable range. Specifically, it is more preferable to satisfy M ⁇ L ⁇ 20, and it is more preferable to satisfy M ⁇ L ⁇ 15.
- M ⁇ H ⁇ 25 may be satisfied. Since the relationship of L ⁇ H is always satisfied, when M ⁇ H ⁇ 25 is satisfied, M ⁇ L ⁇ 25 is also satisfied. It is more preferable to satisfy M ⁇ H ⁇ 20, and it is more preferable to satisfy M ⁇ H ⁇ 15.
- M ⁇ N ⁇ 25 may be satisfied. Since the relationship of L ⁇ N is always satisfied, when M ⁇ N ⁇ 25 is satisfied, M ⁇ L ⁇ 25 is also satisfied. It is more preferable to satisfy M ⁇ N ⁇ 20, and it is more preferable to satisfy M ⁇ N ⁇ 15.
- the sealing resin composition 30 is used for sealing electronic components such as semiconductor elements, transistors, thyristors, diodes, solid-state imaging elements, capacitors, resistors, and LEDs.
- the sealing resin composition 30 may include one or more of (a) an epoxy resin, (b) a curing agent, (c) an inorganic filler, (d) a curing accelerator, and (e) a coupling agent.
- the sealing resin composition 30 is granular. The bulk density varies depending on the production method, production conditions, and the like, but can be controlled to, for example, 0.5 g / cc to 1.5 g / cc.
- the true specific gravity of the cured product of the sealing resin composition 30 is 1.6 g / cc or more and 2.3 g / cc or less, preferably 1.
- the ratio of particles of 2 mm or more is 3% by mass or less and the ratio of particles of 2 mm or less 1 mm or more is 15% by mass using any particle size distribution adjusting means. More than 50% by mass The proportion of particles less than 1 ⁇ m and 106 ⁇ m or more is 45% by mass or more and 80% by mass or less, and the fine powder having a particle size of less than 106 ⁇ m is 5% by mass or less.
- the proportion of particles less than 2 mm and 1 mm or more is 20 mass% or more and 45 mass% or less
- the proportion of particles less than 1 mm and 106 ⁇ m or more is 50 mass% or more and 75 mass% or less
- the fine powder having a particle size of less than 106 ⁇ m is 3 mass% or less.
- Grain size It may be adjusted to the cloth. Any particle size distribution adjusting means may be used as long as it is known to those skilled in the art, but a pulverization sieving method, a centrifugal milling method, a hot cut method, etc. can be used. A sieving method is preferred. A JIS standard sieve can be used for sieving.
- the bulk density here is a value measured by the following method.
- sealing resin composition 30 each component that can be contained in the sealing resin composition 30 will be described in detail, and then an example of a method for producing the sealing resin composition 30 will be described.
- (a) Epoxy resins are monomers, oligomers, and polymers in general having two or more epoxy groups in one molecule, and the molecular weight and molecular structure thereof are not particularly limited.
- biphenyl type epoxy resins Bisphenol type epoxy resins, bisphenol F type epoxy resins, tetramethylbisphenol F type epoxy resins and other bisphenol type epoxy resins, stilbene type epoxy resins, hydroquinone type epoxy resins and other crystalline epoxy resins
- cresol novolac type epoxy resins phenol novolacs Type epoxy resin
- novolak type epoxy resin such as naphthol novolak type epoxy resin, phenol aralkyl type epoxy resin containing phenylene skeleton, phenol aralkyl type epoxy resin containing biphenylene skeleton, phenylene bone -Containing naphthol aralkyl epoxy resin, phenol aralkyl epoxy resin such as alkoxynaphthalene skeleton-
- the curing agent is not particularly limited as long as it can be cured by reacting with an epoxy resin.
- an epoxy resin for example, a straight chain having 2 to 20 carbon atoms such as ethylenediamine, trimethylenediamine, tetramethylenediamine, hexamethylenediamine and the like.
- Anili Resol type phenol resins such as modified resole resins and dimethyl ether resole resins
- novolac type phenol resins such as phenol novolak resins, cresol novolak resins, tert-butylphenol novolak resins, nonylphenol novolak resins
- phenylene skeleton containing phenol aralkyl resins, biphenylene skeleton containing phenol aralkyl Phenol aralkyl resins such as resins
- phenol resins having a condensed polycyclic structure such as naphthalene skeleton and anthracene skeleton
- polyoxystyrenes such as polyparaoxystyrene
- HHPA hexahydrophthalic anhydride
- MTHPA methyltetrahydrophthalic anhydride
- Alicyclic acid anhydride trimellitic anhydride (TMA), pyromellitic anhydride (PMDA), benzophenone tetracarboxylic Acid anhydrides including aromatic acid anhydrides such as acids (BTDA); Polymercaptan compounds such as polysulfides, thioesters and thioethers; Isocyanate compounds such as isocyanate prepolymers and blocked isocyanates; Organics such as carboxylic acid-containing polyester resins Acids are exemplified. These may be used alone or in combination of two or more.
- the curing agent used for the semiconductor encapsulating material is preferably a compound having at least two phenolic hydroxyl groups in one molecule from the viewpoint of moisture resistance, reliability, etc., and a phenol novolac resin and cresol novolac.
- Resins tert-butylphenol novolak resins, nonylphenol novolak resins, trisphenol methane novolak resins and other novolak type phenol resins; resol type phenol resins; polyoxystyrenes such as polyparaoxystyrene; phenylene skeleton-containing phenol aralkyl resins, biphenylene skeleton-containing phenol aralkyls Examples thereof include resins and biphenyl aralkyl resins. In addition, it is preferable to use those having a phenylene and / or biphenyl skeleton in the molecular structure and a hydroxyl group equivalent of 160 or more.
- curing agent It is preferable that it is 1.5 mass% or more in all the resin compositions, and it is more preferable that it is 3 mass% or more, More preferably, it is 5 mass% or more. When the lower limit value of the blending ratio is within the above range, sufficient fluidity can be obtained. Further, (b) the upper limit of the blending ratio of the entire curing agent is not particularly limited, but is preferably 20% by mass or less, more preferably 15% by mass or less in the total resin composition, It is more preferable that it is 8 mass% or less. When the upper limit of the blending ratio is within the above range, good solder resistance can be obtained. Moreover, in order to make it hard to produce caking, it is desirable to adjust a compounding ratio suitably according to the kind of hardening
- the blending ratio of the entire epoxy resin and the entire phenol resin curing agent is the number of epoxy groups (EP) of the entire epoxy resin and the phenol resin curing. It is preferable that the equivalent ratio (EP / OH) with the number of phenolic hydroxyl groups (OH) of the whole agent is 0.8 or more and 1.3 or less. When the equivalent ratio is within this range, sufficient curability can be obtained during molding of the resin composition. Moreover, when the equivalent ratio is within this range, good physical properties in the cured resin can be obtained.
- the curing accelerator used is used so that the curability of the resin composition and the glass transition temperature or the thermal elastic modulus of the cured resin can be increased. It is desirable to adjust the equivalent ratio (EP / OH) between the number of epoxy groups (EP) of the entire epoxy resin and the number of phenolic hydroxyl groups (OH) of the entire curing agent (OH) according to the kind of the epoxy resin. In order to improve the meltability, it is desirable to adjust the equivalent ratio as appropriate according to the type of epoxy resin and phenol resin curing agent used.
- the lower limit of the blending ratio in the sealing resin composition of the entire epoxy resin and the entire phenol resin-based curing agent is preferably 3.5% by mass or more, more preferably 7% by mass or more, and more preferably 10% by mass or more.
- the upper limit is preferably 45% by mass or less, more preferably 35% by mass or less, and more preferably 21% by mass or less.
- the inorganic filler is not particularly limited as long as the sealing resin composition 30 has good caking properties, such as fused crushed silica, fused spherical silica, crystalline silica, secondary agglomerated silica and the like.
- Silica Alumina, silicon nitride, aluminum nitride, boron nitride, titanium oxide, silicon carbide, aluminum hydroxide, magnesium hydroxide, titanium white, talc, clay, mica, glass fiber and the like. Among these, silica is particularly preferable, and fused spherical silica is more preferable.
- the shape of the particles is preferably infinitely spherical, and the amount of filling can be increased by mixing particles having different particle sizes. Moreover, in order to improve the meltability of the resin composition, it is preferable to use fused spherical silica.
- the inorganic filler may be mixed with one or more fillers, the entire specific surface area (SSA) is preferable to be below 5 m 2 / g, the lower limit is 0.1 m 2 / g or more is preferable, and 2 m 2 / g or more is more preferable.
- the average particle diameter (D 50 ) of the entire inorganic filler is preferably 1 ⁇ m or more and 30 ⁇ m or less, more preferably 2 ⁇ m or more and 20 ⁇ m or less, and more preferably 5 ⁇ m or more and 20 ⁇ m or less.
- the (c) an inorganic filler, the specific surface area (SSA) and / or the average particle size (D 50) can also be used two or more kinds of (c) an inorganic filler which is different.
- Examples of average particle diameter (D 50) is relatively large (c) an inorganic filler, preferably an average particle size (D 50) 5 ⁇ m or 35 ⁇ m or less, or more preferably 30 ⁇ m or less of spherical silica least 10 [mu] m. Such an average particle size (D 50 ) is relatively large.
- the content of the (c) inorganic filler is preferably 10% by mass or more, more preferably 20% by mass or more, based on the whole (c) inorganic filler. More preferably, it can be 60 mass% or more.
- average particle diameter (D 50) is relatively large (c) an inorganic filler, an average particle diameter (D 50) is at 5 ⁇ m or 35 ⁇ m or less, and any of the following (i) to (v) Examples thereof include fused spherical silica (c1) having a particle size distribution to be satisfied.
- the content of such (c1) fused spherical silica is preferably 10% by mass or more, more preferably 20% by mass or more, and more preferably 60% by mass or more in the (c) inorganic filler. By doing so, the meltability can be further improved.
- the specific surface area is preferably 0.1 m 2 / g or more and 5.0 m 2 / g or less, more preferably 1.5 m 2 / g or more and 5 It is preferable to use spherical silica of 0.0 m 2 / g or less.
- the content of such spherical silica is preferably 10% by mass or more, more preferably 20% by mass or more, and more preferably 60% by mass or more with respect to (c) the entire inorganic filler.
- the average particle diameter (D 50) as an example of a relatively small (c) an inorganic filler preferably include 5 ⁇ m less spherical silica least 0.1 [mu] m.
- the content of the inorganic filler (c) having such a relatively small average particle diameter (D 50 ) is preferably 60% by mass or less, more preferably 45% by mass or less, based on (c) the entire inorganic filler. More preferably, it can be 30 mass% or less.
- Preferred examples of average particle diameter (D 50) is relatively small (c) an inorganic filler, an average particle diameter (D 50) of less than 5 ⁇ m or more 0.1 ⁇ m fused spherical silica (c2), the average particle more preferable examples
- a fused spherical silica (c3) having a diameter (D 50 ) of 0.1 ⁇ m or more and 1 ⁇ m or less and a fused spherical silica (c4) having an average particle diameter (D 50 ) of 1 ⁇ m or more and less than 5 ⁇ m are used alone or in combination. Can be mentioned.
- the specific surface area is 3.0 m 2 / g or more and 10.0 m 2 / g or less, more preferably 3.5 m 2 / g or more and 8 m.
- examples include spherical silica of 2 / g or less. The content of such spherical silica is preferably not more than 80% by mass, more preferably not more than 50% by mass, and more preferably not more than 20% by mass with respect to (c) the whole inorganic filler.
- spherical silica 1 mass% or more 29 wt% or less and wherein the average particle size (D 50) 1 ⁇ m or 5 ⁇ m below (c4) fused spherical silica 1% by weight or more 29 wt% or less, and wherein (c3) fused spherical
- the total amount of silica and (c4) fused spherical silica may be 6 mass% or more and 30 mass% or less.
- the specific surface area (SSA) of the inorganic filler is obtained by measuring with a commercially available specific surface area meter (for example, MACSORB HM-MODEL-1201 manufactured by Mountec Co., Ltd.). .
- a commercially available specific surface area meter for example, MACSORB HM-MODEL-1201 manufactured by Mountec Co., Ltd.
- the average particle diameter (D 50 ) and particle diameter of the inorganic filler were determined by measuring with a commercially available laser particle size distribution meter (for example, SALD-7000 manufactured by Shimadzu Corporation).
- the lower limit of the content of the inorganic filler is preferably 60% by mass or more, more preferably 75% by mass or more based on the entire sealing resin composition 30 of the present embodiment.
- the lower limit of the content of the inorganic filler is within the above range, the cured product physical properties of the resin composition do not increase the amount of moisture absorption or decrease the strength, and have good solder crack resistance. It is possible to obtain the properties and hardly cause caking.
- an upper limit of the content rate of (c) inorganic filler it is preferable that it is 95 mass% or less of the whole resin composition, it is more preferable that it is 92 mass% or less, and it is 90 mass% or less. Particularly preferred.
- (D) Curing accelerator As a hardening accelerator, what is necessary is just to accelerate
- phosphorus-containing compounds such as organic phosphines, tetra-substituted phosphonium compounds, phospho
- a phosphorus atom-containing compound is preferable from the viewpoint of curability, and from the viewpoint of balance between fluidity and curability, a tetra-substituted phosphonium compound, a phosphobetaine compound, an adduct of a phosphine compound and a quinone compound, a phosphonium compound A curing accelerator having a latent property such as an adduct of silane compound is more preferable. In view of fluidity, tetra-substituted phosphonium compounds are particularly preferable.
- phosphobetaine compounds, adducts of phosphine compounds and quinone compounds are particularly preferable, and in view of latent curability.
- An adduct of a phosphonium compound and a silane compound is particularly preferable.
- a tetra-substituted phosphonium compound is preferable.
- organic phosphine and nitrogen atom-containing compounds are also preferably used.
- Examples of the organic phosphine that can be used in the sealing resin composition 30 according to the present embodiment include a first phosphine such as ethylphosphine and phenylphosphine; a second phosphine such as dimethylphosphine and diphenylphosphine; trimethylphosphine, triethylphosphine, Third phosphine such as tributylphosphine and triphenylphosphine can be used.
- a first phosphine such as ethylphosphine and phenylphosphine
- a second phosphine such as dimethylphosphine and diphenylphosphine
- trimethylphosphine triethylphosphine
- Third phosphine such as tributylphosphine and triphenylphosphine can be used.
- Examples of the tetra-substituted phosphonium compound that can be used in the epoxy resin composition according to this embodiment include a compound represented by the following general formula (1).
- P represents a phosphorus atom
- R1, R2, R3 and R4 each independently represents an aromatic group or an alkyl group
- A represents a functional group selected from a hydroxyl group, a carboxyl group and a thiol group.
- AH is an aromatic organic having at least one functional group selected from a hydroxyl group, a carboxyl group, and a thiol group in the aromatic ring
- x and y are numbers from 1 to 3
- z is a number from 0 to 3
- x y.
- the compound represented by the general formula (1) is obtained, for example, as follows, but is not limited thereto. First, a tetra-substituted phosphonium halide, an aromatic organic acid and a base are mixed in an organic solvent and mixed uniformly to generate an aromatic organic acid anion in the solution system. Next, when water is added, the compound represented by the general formula (1) can be precipitated.
- R1, R2, R3, and R4 bonded to the phosphorus atom are phenyl groups, and AH is bonded to the phosphorus atom from the viewpoint of excellent balance between the yield during synthesis and the curing acceleration effect.
- a compound having a hydroxyl group in an aromatic ring that is, a phenol compound
- A is preferably an anion of the phenol compound.
- Phenol compounds are monocyclic phenol, cresol, catechol, resorcin, condensed polycyclic naphthol, dihydroxynaphthalene, (polycyclic) bisphenol A, bisphenol F, bisphenol S, biphenol having a plurality of aromatic rings. , Phenylphenol, phenol novolac and the like, and among them, phenol compounds having two hydroxyl groups are preferably used.
- Examples of the phosphobetaine compound that can be used in the epoxy resin composition according to this embodiment include a compound represented by the following general formula (2).
- P represents a phosphorus atom
- O represents an oxygen atom
- X1 represents an alkyl group having 1 to 3 carbon atoms
- Y1 represents a hydroxyl group
- a is a number from 0 to 5.
- B is a number from 0 to 4.
- the compound represented by the general formula (2) is obtained, for example, as follows. First, it is obtained through a step of bringing a triaromatic substituted phosphine, which is a third phosphine, into contact with a diazonium salt and replacing the triaromatic substituted phosphine with a diazonium group of the diazonium salt.
- a triaromatic substituted phosphine which is a third phosphine
- the present invention is not limited to this.
- Examples of the adduct of a phosphine compound and a quinone compound that can be used in the epoxy resin composition according to this embodiment include compounds represented by the following general formula (3).
- P represents a phosphorus atom
- O represents an oxygen atom
- OH represents a hydroxy group
- R5, R6, and R7 are each independently an alkyl group having 1 to 12 carbon atoms or a carbon atom
- R 8 and R 10 each independently represents a hydrogen atom or a hydrocarbon group having 1 to 12 carbon atoms, and R 8 and R 9 are bonded to each other to form a ring. May be.
- Examples of the phosphine compound used as an adduct of a phosphine compound and a quinone compound include an aromatic ring such as triphenylphosphine, tris (alkylphenyl) phosphine, tris (alkoxyphenyl) phosphine, trinaphthylphosphine, and tris (benzyl) phosphine.
- aromatic ring such as triphenylphosphine, tris (alkylphenyl) phosphine, tris (alkoxyphenyl) phosphine, trinaphthylphosphine, and tris (benzyl) phosphine.
- Those having a substituent or a substituent such as an alkyl group or an alkoxyl group are preferred.
- Examples of the substituent such as an alkyl group and an alkoxyl group include those having 1 to 6 carbon atoms. From the viewpoint of availability, tripheny
- examples of the quinone compound used for the adduct of the phosphine compound and the quinone compound include o-benzoquinone, p-benzoquinone and anthraquinones, and among them, p-benzoquinone is preferable from the viewpoint of storage stability.
- the adduct can be obtained by contacting and mixing in a solvent capable of dissolving both organic tertiary phosphine and benzoquinone.
- the solvent is preferably a ketone such as acetone or methyl ethyl ketone, which has low solubility in the adduct.
- the present invention is not limited to this.
- R5, R6 and R7 bonded to the phosphorus atom are phenyl groups, and R8, R9 and R10 are hydrogen atoms, that is, 1,4-benzoquinone and triphenyl
- R5, R6 and R7 bonded to the phosphorus atom are phenyl groups
- R8, R9 and R10 are hydrogen atoms, that is, 1,4-benzoquinone and triphenyl
- the compound to which phosphine is added is preferable in that it reduces the thermal elastic modulus of the cured epoxy resin composition.
- Examples of the adduct of a phosphonium compound and a silane compound that can be used in the epoxy resin composition according to this embodiment include a compound represented by the following formula (4).
- P represents a phosphorus atom
- Si represents a silicon atom
- R11, R12, R13 and R14 each independently represent an organic group having an aromatic ring or a heterocyclic ring, or an aliphatic group
- X2 is an organic group bonded to the groups Y2 and Y3.
- X3 is an organic group bonded to the groups Y4 and Y5.
- Y2 and Y3 represent a group formed by releasing a proton from a proton donating group, and groups Y2 and Y3 in the same molecule are bonded to a silicon atom to form a chelate structure.
- Y4 and Y5 represent a group formed by releasing a proton from a proton donating group, and groups Y4 and Y5 in the same molecule are bonded to a silicon atom to form a chelate structure.
- X2 and X3 may be the same or different from each other, and Y2, Y3, Y4, and Y5 may be the same or different from each other.
- Z1 is an organic group having an aromatic ring or a heterocyclic ring, or an aliphatic group.
- examples of R11, R12, R13, and R14 include phenyl group, methylphenyl group, methoxyphenyl group, hydroxyphenyl group, naphthyl group, hydroxynaphthyl group, benzyl group, methyl group, ethyl group, n-butyl group, n-octyl group, cyclohexyl group, and the like.
- an aromatic group having a substituent such as phenyl group, methylphenyl group, methoxyphenyl group, hydroxyphenyl group, hydroxynaphthyl group, or the like.
- a substituted aromatic group is more preferred.
- the groups represented by -Y2-X2-Y3- and -Y4-X3-Y5- in general formula (4) are composed of groups in which the proton donor releases two protons.
- the proton donor is preferably an organic acid having at least two carboxyl groups or hydroxyl groups in the molecule, and further an aromatic group having at least two carboxyl groups or hydroxyl groups on the carbon constituting the aromatic ring.
- a compound is preferable, and an aromatic compound having at least two hydroxyl groups on adjacent carbons constituting an aromatic ring is more preferable.
- catechol pyrogallol, 1,2-dihydroxynaphthalene, 2,3-dihydroxynaphthalene, 2,2′-biphenol, 1,1′-bi-2-naphthol, salicylic acid, 1-hydroxy-2-naphthoic acid, 3 -Hydroxy-2-naphthoic acid, chloranilic acid, tannic acid, 2-hydroxybenzyl alcohol, 1,2-cyclohexanediol, 1,2-propanediol, glycerin and the like.
- catechol, 1,2-dihydroxynaphthalene, and 2,3-dihydroxynaphthalene are more preferable from the viewpoint of easy availability of raw materials and a curing acceleration effect.
- Z1 in the general formula (4) represents an organic group or an aliphatic group having an aromatic ring or a heterocyclic ring. Specific examples thereof include a methyl group, an ethyl group, a propyl group, a butyl group, and a hexyl group.
- Reactions such as aliphatic hydrocarbon groups such as octyl group and aromatic hydrocarbon groups such as phenyl group, benzyl group, naphthyl group and biphenyl group, glycidyloxypropyl group, mercaptopropyl group, aminopropyl group and vinyl group Among them, a methyl group, an ethyl group, a phenyl group, a naphthyl group, and a biphenyl group are more preferable from the viewpoint of thermal stability.
- a silane compound such as phenyltrimethoxysilane and a proton donor such as 2,3-dihydroxynaphthalene are added to a flask containing methanol, and then dissolved.
- Sodium methoxide-methanol solution is added dropwise with stirring.
- crystals are precipitated. The precipitated crystals are filtered, washed with water, and vacuum dried to obtain an adduct of a phosphonium compound and a silane compound.
- the lower limit of the blending ratio of the entire curing accelerator is preferably 0.1% by mass or more in the total resin composition.
- Sufficient curability can be obtained when the lower limit of the blending ratio of the entire curing accelerator is within the above range.
- the upper limit of the mixture ratio of the whole hardening accelerator is 1 mass% or less in all the resin compositions.
- Sufficient fluidity liquidity can be obtained as the upper limit of the mixture ratio of the whole hardening accelerator is in the said range. In order to improve the meltability, it is desirable to adjust the blending ratio as appropriate according to the type of curing accelerator used.
- (E) Coupling agent various known silane compounds such as epoxy silane, mercapto silane, amino silane, alkyl silane, ureido silane, vinyl silane, titanium compounds, aluminum chelates, aluminum / zirconium compounds, etc.
- An agent can be used. Examples include vinyltrichlorosilane, vinyltrimethoxysilane, vinyltriethoxysilane, vinyltris ( ⁇ -methoxyethoxy) silane, ⁇ -methacryloxypropyltrimethoxysilane, ⁇ - (3,4-epoxycyclohexyl) ethyltrimethoxy.
- the blending amount of the coupling agent is preferably 0.05% by mass or more and 3% by mass or less, and more preferably 0.1% by mass or more and 2.5% by mass or less with respect to (c) the inorganic filler. .
- frame can be adhere
- a colorant such as carbon black; natural wax, synthetic wax, higher fatty acid or metal salt thereof, paraffin, oxidized polyethylene, etc. Release agents; low stress agents such as silicone oil and silicone rubber; ion scavengers such as hydrotalcite; flame retardants such as aluminum hydroxide; various additives such as antioxidants can be blended.
- the glass transition temperature (that is, the glass transition temperature of the composition before curing) of the encapsulating resin composition of the present embodiment obtained by the production method described below using the preferred components described above as appropriate is 15 ° C. or higher. 30 degrees C or less is preferable. By setting it within the above range, it is difficult to consolidate, and it is possible to have a preferable aspect of being quickly melted on a mold.
- the glass transition temperature of the encapsulating resin composition was measured at 5 ° C./min under the atmosphere using a temperature-modulated differential scanning calorimeter (hereinafter referred to as modulated DSC or MDSC), and the value was determined according to JISK7121. .
- modulated DSC temperature-modulated differential scanning calorimeter
- the sealing resin composition 30 of the present embodiment can be granulated by mixing and kneading the above components, and then combining various methods such as pulverization, granulation, extrusion cutting, and sieving alone or in combination.
- a kneader such as a roll, a kneader, or an extruder
- the inside of a rotor composed of a cylindrical outer peripheral portion having a plurality of small holes and a disk-shaped bottom surface
- a method in which a melt-kneaded resin composition is supplied and the resin composition is obtained by passing through small holes by centrifugal force obtained by rotating a rotor (centrifugal milling method); , Cooling and pulverization process to obtain a pulverized product by removing coarse particles and fine powder using a sieve (pulverization sieving method)
- after mixing each raw material component with a mixer screw tip Heating and kn
- thermoforming Method obtained by cutting with a cutter , Also referred to as a "hot-cut method”.), And the like.
- desired particle size distribution and bulk density can be obtained by selecting kneading conditions, centrifugal conditions, sieving conditions, cutting conditions and the like.
- the centrifugal milling method is described in, for example, JP 2010-159400 A.
- the encapsulating resin composition 30 is directly accommodated in the inner packaging material 20.
- the inner packaging material 20 may be a bag such as a plastic bag (eg, polyethylene bag) or a paper bag, or may be a plastic container or a metal container having a predetermined strength.
- the inner packaging material 20 may be made of polyethylene, for example.
- the polyethylene may have a moisture permeability of 5 g / m 2 ⁇ day to 20 g / m 2 ⁇ day.
- the inner packaging material 20 is sealed.
- the means for sealing is not particularly limited, and any conventional means can be used.
- the outer packaging material 10 accommodates the inner packaging material 20 that contains the sealing resin composition 30 and is sealed. Moreover, the sealing resin composition 30 may be accommodated directly in the outer packaging material 10.
- the outer packaging material 10 can be a container having a predetermined strength, such as a metal can or a cardboard box.
- a usage mode of the outer packaging material 10 a case where a plurality of outer packaging materials 10 are stacked in multiple stages, or another article or the like is stacked on the outer packaging material 10 can be considered. Assuming such a mode of use, the outer packaging material 10 does not greatly deform even when an article having a predetermined weight (design matter) is laminated, and the weight of the article is within the outer packaging material 10. It is preferable to have a strength that does not affect the encapsulating sealing resin composition 30.
- ⁇ Packing method> As shown in FIG. 1, in this embodiment, after the sealing resin composition 30 is accommodated in the inner packaging material 20 and sealed, the inner packaging material 20 is accommodated in the outer packaging material 10. And when the bulk density of the sealing resin composition 30 is M (g / cc) and the height of the deposit by the sealing resin composition 30 in the state accommodated in the packaging material is L (cm), M ⁇ L ⁇ 25 is satisfied. In the present embodiment, the effect is more remarkable particularly in the sealing resin composition 30 having a bulk density of 0.8 g / cc to 1.4 g / cc, preferably 0.9 g / cc to 1.3 g / cc. It becomes.
- the height L (cm) of the deposit is controlled based on the bulk density M of the sealing resin composition 30 determined based on the required performance. Specifically, the upper limit of the height L (cm) of the deposit is controlled so as to satisfy M ⁇ L ⁇ 25.
- the height L is 27 cm or less, preferably 25 cm or less, more preferably 22 cm or less, and more preferably 15 cm or less.
- Control of the upper limit of the height L (cm) of the granular encapsulating resin composition 30 can be realized by adjusting the shape and size of the space for accommodating the encapsulating resin composition 30, the amount to be accommodated, and the like.
- the upper limit of the height H (cm) of the inner packaging material 20 may be controlled (L ⁇ H).
- the height H is adjusted to 27 cm or less, preferably 25 cm or less, more preferably 22 cm or less, and more preferably 15 cm or less.
- the heights H and N mean the height in a state in which the predetermined surface of the inner packaging material 20 and / or the outer packaging material 10 is placed on the ground surface in accordance with normal practice (the same applies to the following).
- information characters, symbols, etc.
- it means the height in a state where the packaging material is placed on the ground according to the information.
- the pattern which consists of a character, a figure, etc. is attached
- the height in the state which mounted the packaging material on the ground so that the said pattern may be correct up and down is meant.
- the gravity direction is set to the downward direction and the opposite direction is set to the upward direction in view of the effects of this embodiment in the physical distribution and storage processes.
- the height is measured upward from the lower end of the packaging material and the relationship of M ⁇ H ⁇ 25 is satisfied, it is within the range of the present embodiment.
- action of drying or oxygen absorption in the inner side packaging material 20 of the packaging method of this embodiment, such as the said packaging method, or the space between the outer side packaging material 10 and the inner side packaging material 20 is this book. It can also provide with the method which does not impair the effect of embodiment.
- one inner packaging material 20 is accommodated in one outer packaging material 10.
- a plurality of inner packaging materials 20 can be accommodated in one outer packaging material 10.
- the inside of the outer packaging material 10 may be divided into a plurality of rooms by a partition 11 extending in the height direction of the outer packaging material 10.
- a plurality of inner packaging materials 20 may be individually accommodated in a plurality of rooms.
- the inside of the outer packaging material 10 is divided into four rooms, the number is not particularly limited.
- the shape of each room is a quadrangular prism, but is not limited to this, and may be a triangular prism or the like.
- the sealing resin composition 30 is packed so as to satisfy M ⁇ L ⁇ 25.
- you may pack the sealing resin composition 30 so that MxH ⁇ 25 may be satisfy
- you may pack the sealing resin composition 30 so that MxN ⁇ 25 may be satisfy
- the inside of the outer packaging material 10 is divided into a plurality of rooms (partitioned vertically) with a partition 12 extending in a direction substantially perpendicular to the height direction of the outer packaging material 10. )
- a plurality of inner packaging materials 20 may be individually accommodated in a plurality of rooms.
- the inside of the outer packaging material 10 is divided into two rooms, the number is not particularly limited.
- the weight of the inner packaging material 20 accommodated in the upper chamber is set to the lower side. It is preferable to provide an upper stage supporting means that does not cover the sealing resin composition 30 in the inner packaging material 20 accommodated in the room.
- the configuration of the upper support means is not particularly limited.
- the upper support means may be realized by bases 13 having predetermined heights provided at the four corners of the outer packaging material 10.
- the partition 12 is supported by being placed on the base 13.
- the partition 12 and the base 13 are comprised in the intensity
- the base 13 may be provided at a position other than the four corners of the outer packaging material 10.
- the sealing resin composition when the weight of the inner packaging material 20 accommodated in the upper chamber is not applied to the sealing resin composition 30 in the inner packaging material 20 accommodated in the lower chamber, the sealing resin composition
- the height L (cm) of the deposit by the object 30 is the height of the deposit of each sealing resin composition 30 in the inner packaging material 20 accommodated in each room.
- the sealing resin composition 30 is packed so as to satisfy M ⁇ L ⁇ 25.
- you may pack the sealing resin composition 30 so that MxH ⁇ 25 may be satisfy
- you may pack the sealing resin composition 30 so that MxN ⁇ 25 may be satisfy
- the height N of the space for accommodating the inner packaging material 20 formed by the outer packaging material 10 means the height of each room for accommodating the inner packaging material 20.
- the inside of the outer packaging material 10 is divided into a partition 11 extending in the height direction of the outer packaging material 10 and a partition 12 extending in a direction perpendicular to the height direction. It may be divided into a plurality of rooms. And you may accommodate the inner side packaging material 20 (not shown) in each of several chambers. In FIG. 4, the inside of the outer packaging material 10 is divided into eight rooms, but the number is not particularly limited. Also in this modification, it is preferable to provide the upper stage support means, but it is omitted in FIG.
- the sealing resin composition 30 is packed so as to satisfy M ⁇ L ⁇ 25.
- you may pack the sealing resin composition 30 so that MxH ⁇ 25 may be satisfy
- you may pack the sealing resin composition 30 so that MxN ⁇ 25 may be satisfy
- the height N of the space for accommodating the inner packaging material 20 formed by the outer packaging material 10 means the height of each room for accommodating the inner packaging material 20.
- the maximum value of the self-gravity can be limited to a desired range even if any of the plurality of outer surfaces of the outer packaging material 10 is placed on the ground as the bottom surface.
- the height of the inner packaging material 20 in a state where each surface different from the bottom surface of the outer packaging material 10 according to normal practice is placed on the ground is H ′
- M ⁇ H ′ ⁇ 25 is satisfied.
- the height of the space for accommodating the inner packaging material 20 formed by the outer packaging material 10 in a state where each surface different from the bottom surface of the outer packaging material 10 according to normal practice is placed on the ground is defined as N. If ′, the design is made to satisfy M ⁇ N ′ ⁇ 25.
- the height N (cm) of each room is adjusted to satisfy M ⁇ N ⁇ 25. In addition, even when any of the plurality of outer surfaces of the outer packaging material 10 is placed on the ground as the bottom surface, the height of each room N (cm) may be adjusted to satisfy M ⁇ N ⁇ 25. Good.
- the inside of the outer packaging material 10 may be divided into a plurality of rooms so as to be multistage.
- the outer packaging material 10 is configured so that the weight of the sealing resin composition 30 accommodated in a room does not apply to the sealing resin composition 30 accommodated in another room.
- Such a configuration can be realized by using the example described above (an example using the upper support means) or the like.
- FIGS. 1-10 Schematic diagrams of the weighing method of the granular sealing resin composition and the method for supplying it to the mold cavity are shown in FIGS.
- the resin material supply container 102 having a resin material supply mechanism such as a shutter that can instantaneously supply the sealing resin composition 30 into the lower mold cavity 104
- the encapsulating resin composition 30 is granulated using a conveying means such as a vibration feeder 101.
- a predetermined amount of the sealing resin composition 30 is conveyed to prepare a resin material supply container 102 in which the granular sealing resin composition 30 is placed (see FIG. 5).
- the granular sealing resin composition 30 in the resin material supply container 102 can be measured by a measuring means installed under the resin material supply container 102.
- the problem of agglomerates caused by caking that is important in the present embodiment occurs in this step.
- the granular sealing resin composition may not be smoothly flowed during transportation or may be consolidated easily.
- a lump has already occurred, or a lump or a part of the granule is left untransferred on the resin material supply container during the conveyance with the vibration feeder 101 or the like, resulting in a lump.
- the resin material supply container 102 in which the granular sealing resin composition 30 is placed is placed between the upper mold and the lower mold of the compression mold, and the lead frame or circuit board on which the semiconductor element is mounted is mounted.
- the semiconductor element mounting surface is fixed to the upper mold of the compression mold by a fixing means such as clamp and suction (not shown).
- a fixing means such as clamp and suction (not shown).
- the surface opposite to the semiconductor element mounting surface is backed by using a film or the like.
- the weighed granular sealing resin composition 30 is supplied into the lower mold cavity 104 by a resin material supply mechanism such as a shutter constituting the bottom surface of the resin material supply container 102 (see FIG. 6), the granular shape is obtained.
- the sealing resin composition 30 is melted in the lower mold cavity 104 at a predetermined temperature.
- the mold is clamped by a compression molding machine while reducing the pressure inside the cavity as necessary, and the molten sealing resin composition surrounds the semiconductor element.
- the semiconductor element is encapsulated by filling the cavity and curing the encapsulating resin composition for a predetermined time.
- the agglomerate that has already occurred is placed on the mold, or the agglomerate is generated during transfer. Becomes non-uniform, and the wire deformation increases at the portion where it does not melt sufficiently.
- the mold is opened and the semiconductor device is taken out. It is not essential to perform deaeration molding under reduced pressure in the cavity, but it is preferable because voids in the cured product of the sealing resin composition can be reduced.
- the semiconductor element mounted on the lead frame or the circuit board may be plural, and may be stacked or mounted in parallel.
- the sealing resin composition is reduced on the mold and reduced in caking trouble when the sealing resin composition is conveyed and measured in the molding machine. It has an excellent effect in suppressing wire deformation caused by unevenness of objects.
- the semiconductor element sealed by the semiconductor device of this embodiment is not particularly limited, and examples thereof include an integrated circuit, a large-scale integrated circuit, a transistor, a thyristor, a diode, and a solid-state imaging element.
- the form of the semiconductor device of the present embodiment is not particularly limited, and examples thereof include a ball grid array (BGA), a MAP type BGA, and the like. Also applicable to chip size package (CSP), quad flat non-ready package (QFN), small outline non-ready package (SON), lead frame BGA (LF-BGA), etc. .
- BGA ball grid array
- CSP chip size package
- QFN quad flat non-ready package
- SON small outline non-ready package
- LF-BGA lead frame BGA
- the semiconductor device of this embodiment in which the semiconductor element is encapsulated with a cured product of the encapsulating resin composition by compression molding is completed as it is or at a temperature of about 80 ° C. to 200 ° C., taking about 10 minutes to 10 hours. After curing, it is mounted on an electronic device or the like.
- a lead frame or a circuit board one or more semiconductor elements stacked or mounted in parallel on the lead frame or the circuit board, and bonding wires for electrically connecting the lead frame or the circuit board and the semiconductor element
- a semiconductor device including a semiconductor element and a sealing material for sealing a bonding wire will be described in detail with reference to the drawings.
- the present embodiment is not limited to the one using a bonding wire.
- FIG. 7 is a diagram showing a cross-sectional structure of an example of a semiconductor device obtained by sealing a semiconductor element mounted on a lead frame using the sealing resin composition 30 according to the present embodiment.
- a semiconductor element 401 is fixed on the die pad 403 through a die bond material cured body 402.
- the electrode pad of the semiconductor element 401 and the lead frame 405 are connected by a wire 404.
- the semiconductor element 401 is sealed with a sealing material 406 made of a cured body of the sealing resin composition 30 of this embodiment.
- FIG. 8 is a view showing a cross-sectional structure of an example of a semiconductor device obtained by sealing a semiconductor element mounted on a circuit board using the sealing resin composition 30 according to the present embodiment.
- a semiconductor element 401 is fixed on a circuit board 408 through a die bond material cured body 402.
- the electrode pad of the semiconductor element 401 and the electrode pad on the circuit board 408 are connected by a wire 404. Only one side of the circuit board 408 on which the semiconductor element 401 is mounted is sealed with a sealing material 406 formed of a cured body of the sealing resin composition 30 of the present embodiment.
- the electrode pad 407 on the circuit board 408 is bonded to the solder ball 409 on the non-sealing surface side on the circuit board 408 inside.
- the sealing resin composition 30 of the present embodiment is not limited to a semiconductor element such as an integrated circuit or a large-scale integrated circuit, but various elements such as a transistor, a thyristor, a diode, a solid-state imaging element, a capacitor, a resistor, An LED or the like can be sealed.
- Second Embodiment The present inventor has intensively studied the prevention of mutual adhesion of epoxy resin particles for sealing, and the powder glass transition of an epoxy resin composition (epoxy resin composition for sealing) measured using a temperature-modulated differential scanning calorimeter. It was further found that the scale of temperature is effective as a design guideline for satisfying the conditions 1 and 2 described above. Hereinafter, this embodiment will be described.
- the granular epoxy resin composition for sealing according to this embodiment has a granular glass transition temperature of 12 ° C. or more and 35 ° C. or less measured using a temperature-modulated differential scanning calorimeter (Modulated Differential Scanning Calorimetry: MDSC). is there. Condition 1 and condition 2 are easily satisfied when the powder glass transition temperature is in this range.
- the granular glass transition temperature measured using a temperature-modulated differential scanning calorimeter is a measure showing the mutual adhesion prevention property of the granular epoxy resin composition for sealing.
- This temperature modulation differential scanning calorimeter is a measuring method in which the temperature is increased by applying a sine wave temperature modulation simultaneously with the constant temperature increase. For this reason, unlike the conventional differential scanning calorimeter, it becomes possible to measure the heat flow corresponding to the specific heat change, and it becomes possible to evaluate the mutual adhesion prevention property of the resin composition more precisely.
- condition 1 and condition 2 are easily satisfied.
- the granular glass transition temperature measured using a temperature modulation differential scanning calorimeter can be specifically measured as follows.
- the powder glass transition temperature was measured using a temperature-modulated differential scanning calorimeter at 5 ° C./min under an air stream, and the value was determined according to JIS K7121.
- the epoxy resin composition for sealing according to the present embodiment is controlled by controlling the content of particles having a specific size in the particle size distribution measured by sieving using a JIS standard sieve. It is possible to further improve the mutual adhesion prevention property.
- the content of particles having a particle diameter of 2 mm or more is compared with the sealing epoxy resin composition according to this embodiment. It is preferable that it is 3 mass% or less. By controlling the amount within this range, the mutual adhesion prevention property can be further improved.
- the content of particles having a particle size of 2 mm or more is more preferably 1.5% by mass or less.
- the content of fine powder with a particle size of less than 106 ⁇ m in the particle size distribution of the epoxy resin composition for sealing measured by sieving using a JIS standard sieve of 150 mesh is also included in the epoxy resin composition for sealing according to this embodiment. It is preferable that it is 5 mass% or less with respect to it. By controlling the amount within this range, the mutual adhesion prevention property can be further improved. In addition, it is more preferable that content of the fine powder having a particle size of less than 106 ⁇ m is 3% by mass or less.
- the ratio of particles of 2 mm or more is 3% by mass or less, and the ratio of particles of less than 2 mm and 1 mm or more is 15% by mass or more and 50% by mass or less, 1 mm.
- the ratio of particles having a particle size of less than 106 ⁇ m is 45% by mass or more and 80% by mass or less, and the fine powder having a particle size of less than 106 ⁇ m is 5% by mass or less, preferably the ratio of particles of 2 mm or more is 1.5% by mass or less and less than 2 mm and 1 mm or more.
- the proportion of particles is 20% by mass or more and 45% by mass or less, and the proportion of particles less than 1 mm of 106 ⁇ m or more is adjusted to a particle size distribution of 50% by mass or more and 75% by mass or less and fine powder having a particle size of less than 106 ⁇ m is 3% by mass or less. .
- the sealing resin composition 30 of the present embodiment includes (a) an epoxy resin, (b) a curing agent, and (c) an inorganic filler as essential components, but (d) a curing accelerator and (e) a coupling. An agent may further be included.
- each component will be specifically described.
- An epoxy resin can be made the same as in the first embodiment, except for the blending ratio.
- the lower limit of the blending ratio of the entire epoxy resin is not particularly limited, but it is preferably 2% by mass or more, more preferably 4% by mass or more in the total resin composition. When the lower limit of the blending ratio is within the above range, there is little possibility of causing a decrease in fluidity. Moreover, although it does not specifically limit about (a) the upper limit of the mixture ratio of the whole epoxy resin, It is preferable that it is 22 mass% or less in all the resin compositions, and it is more preferable that it is 20 mass% or less.
- the upper limit value of the blending ratio is within the above range, there is little decrease in the powder glass transition temperature, mutual adhesion can be appropriately suppressed, and there is little possibility of causing a decrease in solder resistance and the like.
- the lower limit of the blending ratio of the entire curing agent is not particularly limited, but is preferably 2% by mass or more and more preferably 3% by mass or more in the total resin composition. When the lower limit value of the blending ratio is within the above range, sufficient fluidity can be obtained. Moreover, although it does not specifically limit about the upper limit of the compounding ratio of the whole (b) hardening
- the total number of epoxy groups (EP) of the entire epoxy resin and the entire phenol resin-based curing agent are used as a blending ratio of the entire epoxy resin and the entire phenol resin-based curing agent.
- the equivalent ratio (EP / OH) to the number of phenolic hydroxyl groups (OH) is preferably 0.8 or more and 1.3 or less. When the equivalent ratio is within this range, sufficient curability can be obtained during molding of the resin composition. Moreover, when the equivalent ratio is within this range, good physical properties in the cured resin can be obtained.
- the curing accelerator used is used so that the curability of the resin composition and the glass transition temperature or the thermal elastic modulus of the cured resin can be increased. It is desirable to adjust the equivalent ratio (EP / OH) between the number of epoxy groups (EP) of the entire epoxy resin and the number of phenolic hydroxyl groups (OH) of the entire curing agent (OH) according to the kind of the epoxy resin. In order to improve the meltability, it is desirable to adjust the equivalent ratio as appropriate according to the type of epoxy resin and phenol resin curing agent used.
- the inorganic filler can be configured in the same manner as in the first embodiment except for the content ratio.
- the lower limit value of the content ratio of the inorganic filler is preferably 61% by mass or more, more preferably 65% by mass or more based on the whole sealing epoxy resin composition of the present embodiment.
- the lower limit value of the content ratio of the inorganic filler is within the above range, there is little decrease in the powder glass transition temperature, the mutual adhesion can be appropriately suppressed, and the cured product properties of the resin composition are as follows: Good solder crack resistance can be obtained without increasing the amount of moisture absorption or decreasing the strength.
- an upper limit of the content rate of (c) inorganic filler it is preferable that it is 95 mass% or less of the whole resin composition, it is more preferable that it is 92 mass% or less, and it is 90 mass% or less. Particularly preferred.
- the upper limit value of the content ratio of the inorganic filler is within the above range, the flowability is not impaired and good moldability can be obtained.
- composition of the curing accelerator can be the same as that of the first embodiment.
- a colorant such as carbon black; natural wax, synthetic wax, higher fatty acid or metal salt thereof, paraffin, oxidized polyethylene, etc. Release agents; low stress agents such as silicone oil and silicone rubber; ion scavengers such as hydrotalcite; flame retardants such as aluminum hydroxide; various additives such as antioxidants can be blended.
- the configuration of the stopped semiconductor device is the same as that of the first embodiment.
- the package containing the sealing resin composition 30 in the packaging material (the inner packaging material 20 and / or the outer packaging material 10), and the sealing resin composition
- the invention of the transportation method for transporting the article 30 in a state of being accommodated in the packaging material (the inner packaging material 20 and / or the outer packaging material 10) is also described.
- Epoxy resin 1 Biphenylene skeleton-containing phenol aralkyl epoxy resin (NC3000 manufactured by Nippon Kayaku Co., Ltd.)
- Epoxy resin 2 biphenyl type epoxy resin (manufactured by Japan Epoxy Resin Co., Ltd., YX4000H)
- Phenol resin 1 Biphenylene skeleton-containing phenol aralkyl resin (Maywa Kasei Co., Ltd., MEH-7851SS)
- Phenol resin 2 Phenol aralkyl resin containing phenylene skeleton (Mitsui Chemicals, XLC-4L)
- Spherical inorganic filler 1 spherical fused silica (average particle size 16 ⁇ m, specific surface area 2.1 m 2 / g)
- Spherical inorganic filler 2 Spherical fused silica (average particle size 10 ⁇ m, specific surface area 4.7 m 2 / g)
- Spherical inorganic filler 3 spherical fused silica (average particle size 32 ⁇ m, specific surface area 1.5 m 2 / g)
- Table 1 shows the particle size distribution in the spherical inorganic fillers 1 to 3.
- Fine spherical inorganic filler 1 spherical fused silica (average particle size 0.5 ⁇ m, specific surface area 6.1 m 2 / g)
- Fine spherical inorganic filler 2 spherical fused silica (average particle size 1.5 ⁇ m, specific surface area 4.0 m 2 / g)
- Curing accelerator 1 Triphenylphosphine coupling agent: ⁇ -glycidoxypropyltrimethoxysilane carbon black wax: carnauba wax
- Examples 1, 2, 5> After the raw materials of the epoxy resin composition having the composition shown in Table 2 were pulverized and mixed for 5 minutes by a super mixer, this mixed raw material was screw rotated at 30 RPM at 100 ° C. in a co-rotating twin screw extruder having a cylinder inner diameter of 65 mm. A powdered encapsulating resin composition 30 was obtained by melt-kneading at a resin temperature of 5 ° C. and adjusting the particle size using a sieve after cooling and crushing steps to obtain a pulverized product. Properties of the sealing resin composition 30 are shown in Table 2.
- a plastic bag is used as the inner packaging material 20 in a cardboard case (outer packaging material 10) having a height and width of 32 cm and a height of 28 cm provided with eight rooms by the packing method according to FIG.
- the sealing resin composition 30 obtained above was stored and sealed so that the height of the inner packaging material 20 was the value shown in Table 2, and the cardboard case was closed with gummed tape (this packing method is called A). In Table 2, the same technique is used). After such packaging, it was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left unopened at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours (normal temperature return treatment).
- the height H of the inner packaging material in this example is measured in a state where the packaged sealing resin composition 30 is in contact with the upper surface of the inner packaging material, and is substantially the height H of the inner packaging material.
- the height L of the sealing resin composition 30 can be regarded as equivalent.
- the error between the height L of the sealing resin composition 30 and the height H of the inner packaging material 20 when considering the thickness was several millimeters. .
- the inner packaging material having the same thickness was used, and the height of the inner packaging material 20 was measured in the same manner.
- the sealing resin composition 30 was introduced into a predetermined position of a compression molding machine (PMA1040, manufactured by TOWA Corporation), but no lump was observed. Further, no lump was found in the sealing resin composition 30 conveyed and dispersed on the vibration feeder, the resin material supply container, and the mold, respectively.
- PMA1040 manufactured by TOWA Corporation
- Examples 3 and 4 A sealing resin composition 30 was obtained in the same manner as in Example 1. Properties of the sealing resin composition 30 are shown in Table 2.
- the sealing resin composition obtained above by using a plastic bag as the inner packaging material 20 in a cardboard case (outer packaging material 10) having a length of 32 cm and a height of 20 cm provided with four rooms by a packing method according to FIG. 30 were respectively stored and sealed so that the height of the inner packaging material 20 would be the value shown in Table 2, and the cardboard case was closed with gummed tape (the packaging method of this embodiment is called B, the same applies to Table 2). Notation by technique). After such packaging, it was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left unopened at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours (normal temperature return treatment).
- the sealing resin composition 30 was introduced into a predetermined position of a compression molding machine (PMA1040, manufactured by TOWA Corporation), but no lump was observed. Further, no lump was found in the sealing resin composition 30 conveyed and dispersed on the vibration feeder, the resin material supply container, and the mold, respectively.
- PMA1040 manufactured by TOWA Corporation
- the plastic bag is a cardboard case having a length and width of 32 cm and a height of 35 cm.
- the plastic bags are stored and sealed so that the height of each plastic bag becomes the value shown in Table 2 (the packing method of the comparative example is referred to as C, and the same method is used in Table 2), Similarly to Example 1, room temperature return treatment and molding were performed. As a result, in all cases, a lump was found when the molding machine was introduced, or during conveyance and weighing.
- SSA Specific surface area
- D 50 Average particle size of inorganic filler (D 50 ) SALD-7000 manufactured by Shimadzu Corporation was used and evaluated by a laser diffraction particle size distribution measurement method. D 50 is the median diameter.
- Particle size distribution of encapsulating resin composition granules The particle size distribution was adjusted and determined using JIS standard sieves with mesh openings of 2.00 mm, 1.00 mm, and 0.106 mm provided in a low tap vibrator.
- the obtained sealing resin composition is once compressed into tablets of a predetermined size, using a transfer molding machine, with a mold temperature of 175 ⁇ 5 ° C., an injection pressure of 7 MPa, a curing time of 120 seconds, a diameter of 50 mm ⁇ thickness A disk with a thickness of 3 mm was molded, and the mass and volume were determined to calculate the specific gravity of the cured product.
- the obtained MAP molded product was separated into pieces by dicing to obtain a simulated semiconductor device.
- the soft X-ray device PRO-TEST-100, manufactured by Softex Co., Ltd.
- the wire flow rate in the obtained simulated semiconductor device was measured for the four longest gold wires (length 7 mm) on the diagonal of the package. The average flow rate was measured, and the wire flow rate (wire flow rate / wire length ⁇ 100 (%)) was calculated.
Abstract
Description
顆粒状の封止樹脂組成物を包装資材に収容し、かつ、10℃以下の状態で運搬する前記顆粒状の封止樹脂組成物の運搬方法であって、
前記封止樹脂組成物の嵩密度をM(g/cc)、
前記包装資材内に収容された状態における、前記封止樹脂組成物による堆積物の高さをL(cm)とすると、M×L≦25を満たし、
前記封止樹脂組成物を収容した前記包装資材を、温度4℃、相対湿度35%で24時間放置し、次いで、温度23℃、相対湿度50%で24時間放置した後に前記包装資材から取出した前記封止樹脂組成物は、差角が10度以上となる運搬方法が提供される。 According to the present invention,
The granular sealing resin composition is contained in a packaging material, and the granular sealing resin composition is transported in a state of 10 ° C or less,
The bulk density of the sealing resin composition is M (g / cc),
When the height of the deposit by the sealing resin composition in a state accommodated in the packaging material is L (cm), M × L ≦ 25 is satisfied,
The packaging material containing the sealing resin composition was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours, and then taken out from the packaging material. The encapsulating resin composition is provided with a transport method in which the difference angle is 10 degrees or more.
顆粒状の封止樹脂組成物を包装資材に収容し、かつ、10℃以下の状態で運搬する前記顆粒状の封止樹脂組成物の運搬方法であって、
前記封止樹脂組成物の嵩密度をM(g/cc)、
前記包装資材内に収容された状態における、前記封止樹脂組成物による堆積物の高さをL(cm)とすると、M×L≦25を満たし、
前記封止樹脂組成物を収容した前記包装資材を、温度4℃、相対湿度35%で24時間放置し、次いで、温度23℃、相対湿度50%で24時間放置した後に前記包装資材から取出した前記封止樹脂組成物は、目開き2mmの篩パス品の含有率が90重量%以上となる運搬方法が提供される。 Moreover, according to the present invention,
The granular sealing resin composition is contained in a packaging material, and the granular sealing resin composition is transported in a state of 10 ° C or less,
The bulk density of the sealing resin composition is M (g / cc),
When the height of the deposit by the sealing resin composition in a state accommodated in the packaging material is L (cm), M × L ≦ 25 is satisfied,
The packaging material containing the sealing resin composition was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours, and then taken out from the packaging material. The encapsulating resin composition is provided with a transport method in which the content of a sieve pass product having an opening of 2 mm is 90% by weight or more.
包装資材と、
前記包装資材内に収容された顆粒状の封止樹脂組成物と、
を有し、
前記封止樹脂組成物を収容した前記包装資材を、温度4℃、相対湿度35%で24時間放置し、次いで、温度23℃、相対湿度50%で24時間放置した後に前記包装資材から取出した前記封止樹脂組成物は、差角が10度以上である梱包物が提供される。 Moreover, according to the present invention,
Packaging materials,
A granular sealing resin composition housed in the packaging material;
Have
The packaging material containing the sealing resin composition was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours, and then taken out from the packaging material. The sealing resin composition is provided with a package having a difference angle of 10 degrees or more.
包装資材と、
前記包装資材内に収容された顆粒状の封止樹脂組成物と、
を有し、
前記封止樹脂組成物を収容した前記包装資材を、温度4℃、相対湿度35%で24時間放置し、次いで、温度23℃、相対湿度50%で24時間放置した後に前記包装資材から取出した前記封止樹脂組成物は、目開き2mmの篩パス品の含有率が90重量%以上である梱包物が提供される。 Moreover, according to the present invention,
Packaging materials,
A granular sealing resin composition housed in the packaging material;
Have
The packaging material containing the sealing resin composition was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours, and then taken out from the packaging material. The encapsulating resin composition provides a package in which the content of a sieve pass product having an opening of 2 mm is 90% by weight or more.
まず、本実施形態の概念について説明する。包装資材に収容された顆粒状の封止樹脂組成物(以下、単に「封止樹脂組成物」と言う場合がある)は、その後、様々な場所に運搬されていくが、10℃以下の状態(10℃以下に保たれた空間内に保管された状態)で運搬される場合がある。そして、所定の場所に運搬された後、封止樹脂組成物は室温に戻され、当該状態で使用される。なお、所定の場所に運搬された後、使用されるまでの間、10℃以下の状態で保管される場合がある。 << First Embodiment >>
First, the concept of this embodiment will be described. The granular encapsulating resin composition contained in the packaging material (hereinafter sometimes simply referred to as “encapsulating resin composition”) is then transported to various places, but at a temperature of 10 ° C. or lower. It may be transported in a state where it is stored in a space kept at 10 ° C. or lower. And after conveying to a predetermined place, a sealing resin composition is returned to room temperature and used in the said state. In addition, after being transported to a predetermined place, it may be stored in a state of 10 ° C. or lower until it is used.
封止樹脂組成物30は、半導体素子、トランジスタ、サイリスタ、ダイオード、固体撮像素子、コンデンサ、抵抗、LEDなどの電子部品を封止するために使用される。封止樹脂組成物30は、(a)エポキシ樹脂、(b)硬化剤、(c)無機フィラー、(d)硬化促進剤、(e)カップリング剤の中の一つ以上を含んでもよい。そして、封止樹脂組成物30は顆粒状である。嵩密度は製造方法や製造条件などによりその分布の態様が異なるが、例えば0.5g/cc以上1.5g/cc以下にコントロールすることができる。本発明では特に封止樹脂組成物の嵩密度が0.8g/cc以上1.4g/cc以下、好ましくは0.9g/cc以上1.3g/cc以下の嵩密度の封止樹脂組成物においてその効果がより顕著となる。本実施形態の封止樹脂組成物30が上記の嵩密度を得るには、封止樹脂組成物30の硬化物の真比重が1.6g/cc以上2.3g/cc以下、好ましくは1.8g/cc以上2.1g/cc以下である場合において、任意の粒度分布調整手段を使用して、2mm以上の粒子の割合が3質量%以下、2mm未満1mm以上の粒子の割合が15質量%以上50質量%以下、1mm未満106μm以上の粒子の割合が45質量%以上80質量%以下、粒径106μm未満の微粉が5質量%以下、好ましくは2mm以上の粒子の割合が1.5質量%以下、2mm未満1mm以上の粒子の割合が20質量%以上45質量%以下、1mm未満106μm以上の粒子の割合が50質量%以上75質量%以下、粒径106μm未満の微粉が3質量%以下の粒度分布に調整すればよい。粒度分布調整手段としては、当業者に公知のものであれば何ら差し支えないが、粉砕篩分法、遠心製粉法、ホットカット法などを使用することができ、中でも粒度調整が容易であるので粉砕篩分法が好ましい。篩分けはJIS標準篩を用いることができる。 <Sealing
The sealing
(a)エポキシ樹脂の例は、1分子内にエポキシ基を2個以上有するモノマー、オリゴマー、ポリマー全般であり、その分子量、分子構造を特に限定するものではないが、例えば、ビフェニル型エポキシ樹脂、ビスフェノールA型エポキシ樹脂、ビスフェノールF型エポキシ樹脂、テトラメチルビスフェノールF型エポキシ樹脂などのビスフェノール型エポキシ樹脂、スチルベン型エポキシ樹脂、ハイドロキノン型エポキシ樹脂等の結晶性エポキシ樹脂;クレゾールノボラック型エポキシ樹脂、フェノールノボラック型エポキシ樹脂、ナフトールノボラック型エポキシ樹脂等のノボラック型エポキシ樹脂;フェニレン骨格含有フェノールアラルキル型エポキシ樹脂、ビフェニレン骨格含有フェノールアラルキル型エポキシ樹脂、フェニレン骨格含有ナフトールアラルキル型エポキシ樹脂、アルコキシナフタレン骨格含有フェノールアラルキルエポキシ樹脂等のフェノールアラルキル型エポキシ樹脂;トリフェノールメタン型エポキシ樹脂、アルキル変性トリフェノールメタン型エポキシ樹脂等の3官能型エポキシ樹脂;ジシクロペンタジエン変性フェノール型エポキシ樹脂、テルペン変性フェノール型エポキシ樹脂等の変性フェノール型エポキシ樹脂;トリアジン核含有エポキシ樹脂等の複素環含有エポキシ樹脂等が挙げられ、これらは1種類を単独で用いても2種類以上を組み合わせて用いてもよい。また、分子構造にビフェニル骨格を持ちエポキシ当量が180以上であるものを用いることが好ましい。 [(A) Epoxy resin]
Examples of (a) epoxy resins are monomers, oligomers, and polymers in general having two or more epoxy groups in one molecule, and the molecular weight and molecular structure thereof are not particularly limited. For example, biphenyl type epoxy resins, Bisphenol type epoxy resins, bisphenol F type epoxy resins, tetramethylbisphenol F type epoxy resins and other bisphenol type epoxy resins, stilbene type epoxy resins, hydroquinone type epoxy resins and other crystalline epoxy resins; cresol novolac type epoxy resins, phenol novolacs Type epoxy resin, novolak type epoxy resin such as naphthol novolak type epoxy resin, phenol aralkyl type epoxy resin containing phenylene skeleton, phenol aralkyl type epoxy resin containing biphenylene skeleton, phenylene bone -Containing naphthol aralkyl epoxy resin, phenol aralkyl epoxy resin such as alkoxynaphthalene skeleton-containing phenol aralkyl epoxy resin; trifunctional methane type epoxy resin, trifunctional epoxy resin such as alkyl-modified triphenol methane type epoxy resin; dicyclopentadiene modified Modified phenol type epoxy resins such as phenol type epoxy resins and terpene modified phenol type epoxy resins; and heterocyclic ring containing epoxy resins such as triazine nucleus-containing epoxy resins. These may be used alone or in combination of two or more. You may use it in combination. In addition, it is preferable to use those having a biphenyl skeleton in the molecular structure and an epoxy equivalent of 180 or more.
(b)硬化剤としては、エポキシ樹脂と反応して硬化させるものであれば特に限定されず、例えば、エチレンジアミン、トリメチレンジアミン、テトラメチレンジアミン、ヘキサメチレンジアミン等の炭素数2~20の直鎖脂肪族ジアミン、メタフェニレンジアミン、パラフェニレンジアミン、パラキシレンジアミン、4,4'-ジアミノジフェニルメタン、4,4'-ジアミノジフェニルプロパン、4,4'-ジアミノジフェニルエーテル、4,4'-ジアミノジフェニルスルホン、4,4'-ジアミノジシクロヘキサン、ビス(4-アミノフェニル)フェニルメタン、1,5-ジアミノナフタレン、メタキシレンジアミン、パラキシレンジアミン、1,1-ビス(4-アミノフェニル)シクロヘキサン、ジシアノジアミド等のアミン類;アニリン変性レゾール樹脂やジメチルエーテルレゾール樹脂等のレゾール型フェノール樹脂;フェノールノボラック樹脂、クレゾールノボラック樹脂、tert-ブチルフェノールノボラック樹脂、ノニルフェノールノボラック樹脂等のノボラック型フェノール樹脂;フェニレン骨格含有フェノールアラルキル樹脂、ビフェニレン骨格含有フェノールアラルキル樹脂等のフェノールアラルキル樹脂;ナフタレン骨格やアントラセン骨格のような縮合多環構造を有するフェノール樹脂;ポリパラオキシスチレン等のポリオキシスチレン;ヘキサヒドロ無水フタル酸(HHPA)、メチルテトラヒドロ無水フタル酸(MTHPA)などの脂環族酸無水物、無水トリメリット酸(TMA)、無水ピロメリット酸(PMDA)、ベンゾフェノンテトラカルボン酸(BTDA)などの芳香族酸無水物などを含む酸無水物等;ポリサルファイド、チオエステル、チオエーテルなどのポリメルカプタン化合物;イソシアネートプレポリマー、ブロック化イソシアネートなどのイソシアネート化合物;カルボン酸含有ポリエステル樹脂などの有機酸類が例示される。これらは1種類を単独で用いても2種類以上を組み合わせて用いてもよい。また、これらの内、半導体封止材料に用いる硬化剤としては、耐湿性、信頼性等の点から、1分子内に少なくとも2個のフェノール性水酸基を有する化合物が好ましく、フェノールノボラック樹脂、クレゾールノボラック樹脂、tert-ブチルフェノールノボラック樹脂、ノニルフェノールノボラック樹脂、トリスフェノールメタンノボラック樹脂等のノボラック型フェノール樹脂;レゾール型フェノール樹脂;ポリパラオキシスチレン等のポリオキシスチレン;フェニレン骨格含有フェノールアラルキル樹脂、ビフェニレン骨格含有フェノールアラルキル樹脂、ビフェニルアラルキル樹脂等が例示される。また、分子構造にフェニレン及び/又はビフェニル骨格を持ち水酸基当量が160以上であるものを用いることが好ましい。 [(B) Curing agent]
(B) The curing agent is not particularly limited as long as it can be cured by reacting with an epoxy resin. For example, a straight chain having 2 to 20 carbon atoms such as ethylenediamine, trimethylenediamine, tetramethylenediamine, hexamethylenediamine and the like. Aliphatic diamine, metaphenylenediamine, paraphenylenediamine, paraxylenediamine, 4,4'-diaminodiphenylmethane, 4,4'-diaminodiphenylpropane, 4,4'-diaminodiphenyl ether, 4,4'-diaminodiphenylsulfone, 4,4'-diaminodicyclohexane, bis (4-aminophenyl) phenylmethane, 1,5-diaminonaphthalene, metaxylenediamine, paraxylenediamine, 1,1-bis (4-aminophenyl) cyclohexane, dicyanodiamide, etc. Amines; Anili Resol type phenol resins such as modified resole resins and dimethyl ether resole resins; novolac type phenol resins such as phenol novolak resins, cresol novolak resins, tert-butylphenol novolak resins, nonylphenol novolak resins; phenylene skeleton containing phenol aralkyl resins, biphenylene skeleton containing phenol aralkyl Phenol aralkyl resins such as resins; phenol resins having a condensed polycyclic structure such as naphthalene skeleton and anthracene skeleton; polyoxystyrenes such as polyparaoxystyrene; hexahydrophthalic anhydride (HHPA), methyltetrahydrophthalic anhydride (MTHPA), etc. Alicyclic acid anhydride, trimellitic anhydride (TMA), pyromellitic anhydride (PMDA), benzophenone tetracarboxylic Acid anhydrides including aromatic acid anhydrides such as acids (BTDA); Polymercaptan compounds such as polysulfides, thioesters and thioethers; Isocyanate compounds such as isocyanate prepolymers and blocked isocyanates; Organics such as carboxylic acid-containing polyester resins Acids are exemplified. These may be used alone or in combination of two or more. Of these, the curing agent used for the semiconductor encapsulating material is preferably a compound having at least two phenolic hydroxyl groups in one molecule from the viewpoint of moisture resistance, reliability, etc., and a phenol novolac resin and cresol novolac. Resins, tert-butylphenol novolak resins, nonylphenol novolak resins, trisphenol methane novolak resins and other novolak type phenol resins; resol type phenol resins; polyoxystyrenes such as polyparaoxystyrene; phenylene skeleton-containing phenol aralkyl resins, biphenylene skeleton-containing phenol aralkyls Examples thereof include resins and biphenyl aralkyl resins. In addition, it is preferable to use those having a phenylene and / or biphenyl skeleton in the molecular structure and a hydroxyl group equivalent of 160 or more.
(c)無機フィラーとしては、封止樹脂組成物30としたとき固結性が良好であれば特に制限はなく、例えば、溶融破砕シリカ、溶融球状シリカ、結晶性シリカ、2次凝集シリカ等のシリカ;アルミナ、窒化ケイ素、窒化アルミニウム、窒化ホウ素、酸化チタン、炭化ケイ素、水酸化アルミニウム、水酸化マグネシウム、チタンホワイト、タルク、クレー、マイカ、ガラス繊維等が挙げられる。これらの中でも、特にシリカが好ましく、溶融球状シリカがより好ましい。また、粒子形状は限りなく真球状であることが好ましく、また、粒子の大きさの異なるものを混合することにより充填量を多くすることができる。また、樹脂組成物の融け性を向上させるため、溶融球状シリカを用いるのが好ましい。 [(C) Inorganic filler]
(C) The inorganic filler is not particularly limited as long as the sealing
(ii)粒子径が2μm以下の粒子を7質量%以上11質量%以下含む、
(iii)粒子径が3μm以下の粒子を13質量%以上17質量%以下含む、
(iv)粒子径が48μmを超える粒子を2質量%以上7質量%以下含む、
(v)粒子径が24μmを超える粒子を33質量%以上40質量%以下含む。 (I) particles having a particle diameter of 1 μm or less (c1) 1 to 4.5% by mass based on the whole fused spherical silica,
(Ii) containing 7% by mass to 11% by mass of particles having a particle size of 2 μm or less,
(Iii) 13 to 17% by mass of particles having a particle size of 3 μm or less,
(Iv) 2% by mass or more and 7% by mass or less of particles having a particle diameter exceeding 48 μm;
(V) Containing 33% by mass or more and 40% by mass or less of particles having a particle diameter of more than 24 μm.
(d)硬化促進剤としては、エポキシ基とフェノール性水酸基との硬化反応を促進させるものであればよく、一般に封止材料に使用するものを用いることができる。具体例としては、有機ホスフィン、テトラ置換ホスホニウム化合物、ホスホベタイン化合物、ホスフィン化合物とキノン化合物との付加物、ホスホニウム化合物とシラン化合物との付加物等のリン原子含有化合物;1,8-ジアザビシクロ(5,4,0)ウンデセン-7、イミダゾールなどのアミジン系化合物、ベンジルジメチルアミンなどの3級アミンや前記化合物の4級オニウム塩であるアミジニウム塩、アンモニウム塩などに代表される窒素原子含有化合物が挙げられる。これらのうち、硬化性の観点からはリン原子含有化合物が好ましく、流動性と硬化性のバランスの観点からは、テトラ置換ホスホニウム化合物、ホスホベタイン化合物、ホスフィン化合物とキノン化合物との付加物、ホスホニウム化合物とシラン化合物との付加物等の潜伏性を有する硬化促進剤がより好ましい。流動性という点を考慮するとテトラ置換ホスホニウム化合物が特に好ましく、また耐半田性の観点では、ホスホベタイン化合物、ホスフィン化合物とキノン化合物との付加物が特に好ましく、また潜伏的硬化性という点を考慮すると、ホスホニウム化合物とシラン化合物との付加物が特に好ましい。また、連続成形性の観点では、テトラ置換ホスホニウム化合物が好ましい。また、コスト面を考えると、有機ホスフィン、窒素原子含有化合物も好適に用いられる。 [(D) Curing accelerator]
(D) As a hardening accelerator, what is necessary is just to accelerate | stimulate the hardening reaction of an epoxy group and a phenolic hydroxyl group, and what is generally used for a sealing material can be used. Specific examples include phosphorus-containing compounds such as organic phosphines, tetra-substituted phosphonium compounds, phosphobetaine compounds, adducts of phosphine compounds and quinone compounds, adducts of phosphonium compounds and silane compounds; 1,8-diazabicyclo (5 , 4,0) Undecene-7, amidine compounds such as imidazole, tertiary amines such as benzyldimethylamine, amidinium salts which are quaternary onium salts of the above compounds, and nitrogen atom-containing compounds such as ammonium salts. It is done. Among these, a phosphorus atom-containing compound is preferable from the viewpoint of curability, and from the viewpoint of balance between fluidity and curability, a tetra-substituted phosphonium compound, a phosphobetaine compound, an adduct of a phosphine compound and a quinone compound, a phosphonium compound A curing accelerator having a latent property such as an adduct of silane compound is more preferable. In view of fluidity, tetra-substituted phosphonium compounds are particularly preferable. From the viewpoint of solder resistance, phosphobetaine compounds, adducts of phosphine compounds and quinone compounds are particularly preferable, and in view of latent curability. An adduct of a phosphonium compound and a silane compound is particularly preferable. Further, from the viewpoint of continuous moldability, a tetra-substituted phosphonium compound is preferable. In view of cost, organic phosphine and nitrogen atom-containing compounds are also preferably used.
(e)カップリング剤としては、エポキシシラン、メルカプトシラン、アミノシラン、アルキルシラン、ウレイドシラン、ビニルシラン等の各種シラン系化合物、チタン系化合物、アルミニウムキレート類、アルミニウム/ジルコニウム系化合物等の公知のカップリング剤を用いることができる。これらを例示すると、ビニルトリクロロシラン、ビニルトリメトキシシラン、ビニルトリエトキシシラン、ビニルトリス(β-メトキシエトキシ)シラン、γ-メタクリロキシプロピルトリメトキシシラン、β-(3,4-エポキシシクロヘキシル)エチルトリメトキシシラン、γ-グリシドキシプロピルトリメトキシシラン、γ-グリシドキシプロピルトリエトキシシラン、γ-グリシドキシプロピルメチルジメトキシシラン、γ-メタクリロキシプロピルメチルジエトキシシラン、γ-メタクリロキシプロピルトリエトキシシランビニルトリアセトキシシラン、γ-メルカプトプロピルトリメトキシシラン、γ-アミノプロピルトリエトキシシラン、γ-アニリノプロピルトリメトキシシラン、γ-アニリノプロピルメチルジメトキシシラン、γ-[ビス(β-ヒドロキシエチル)]アミノプロピルトリエトキシシラン、N-β-(アミノエチル)-γ-アミノプロピルトリメトキシシラン、N-β-(アミノエチル)-γ-アミノプロピルトリエトキシシラン、N-β-(アミノエチル)-γ-アミノプロピルメチルジメトキシシラン、N-フェニル-γ-アミノプロピルトリメトキシシラン、γ-(β-アミノエチル)アミノプロピルジメトキシメチルシラン、N-(トリメトキシシリルプロピル)エチレンジアミン、N-(ジメトキシメチルシリルイソプロピル)エチレンジアミン、メチルトリメトキシシラン、ジメチルジメトキシシラン、メチルトリエトキシシラン、N-β-(N-ビニルベンジルアミノエチル)-γ-アミノプロピルトリメトキシシラン、γ-クロロプロピルトリメトキシシラン、ヘキサメチルジシラン、ビニルトリメトキシシラン、γ-メルカプトプロピルメチルジメトキシシラン、3-イソシアネートプロピルトリエトキシシラン、3-アクリロキシプロピルトリメトキシシラン、3-トリエトキシリル-N-(1,3-ジメチルーブチリデン)プロピルアミンの加水分解物等のシラン系カップリング剤、イソプロピルトリイソステアロイルチタネート、イソプロピルトリス(ジオクチルパイロホスフェート)チタネート、イソプロピルトリ(N-アミノエチル-アミノエチル)チタネート、テトラオクチルビス(ジトリデシルホスファイト)チタネート、テトラ(2,2-ジアリルオキシメチル-1-ブチル)ビス(ジトリデシル)ホスファイトチタネート、ビス(ジオクチルパイロホスフェート)オキシアセテートチタネート、ビス(ジオクチルパイロホスフェート)エチレンチタネート、イソプロピルトリオクタノイルチタネート、イソプロピルジメタクリルイソステアロイルチタネート、イソプロピルトリドデシルベンゼンスルホニルチタネート、イソプロピルイソステアロイルジアクリルチタネート、イソプロピルトリ(ジオクチルホスフェート)チタネート、イソプロピルトリクミルフェニルチタネート、テトライソプロピルビス(ジオクチルホスファイト)チタネート等のチタネート系カップリング剤などが挙げられ、これらを単独で用いても2種以上を組み合わせて用いてもよい。 [(E) Coupling agent]
(E) As coupling agents, various known silane compounds such as epoxy silane, mercapto silane, amino silane, alkyl silane, ureido silane, vinyl silane, titanium compounds, aluminum chelates, aluminum / zirconium compounds, etc. An agent can be used. Examples include vinyltrichlorosilane, vinyltrimethoxysilane, vinyltriethoxysilane, vinyltris (β-methoxyethoxy) silane, γ-methacryloxypropyltrimethoxysilane, β- (3,4-epoxycyclohexyl) ethyltrimethoxy. Silane, γ-glycidoxypropyltrimethoxysilane, γ-glycidoxypropyltriethoxysilane, γ-glycidoxypropylmethyldimethoxysilane, γ-methacryloxypropylmethyldiethoxysilane, γ-methacryloxypropyltriethoxysilane Vinyltriacetoxysilane, γ-mercaptopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-anilinopropyltrimethoxysilane, γ-anilinopropylmethyldimethoxysilane, γ [Bis (β-hydroxyethyl)] aminopropyltriethoxysilane, N-β- (aminoethyl) -γ-aminopropyltrimethoxysilane, N-β- (aminoethyl) -γ-aminopropyltriethoxysilane, N -Β- (aminoethyl) -γ-aminopropylmethyldimethoxysilane, N-phenyl-γ-aminopropyltrimethoxysilane, γ- (β-aminoethyl) aminopropyldimethoxymethylsilane, N- (trimethoxysilylpropyl) Ethylenediamine, N- (dimethoxymethylsilylisopropyl) ethylenediamine, methyltrimethoxysilane, dimethyldimethoxysilane, methyltriethoxysilane, N-β- (N-vinylbenzylaminoethyl) -γ-aminopropyltrimethoxysilane, γ-chloro Propyl trimeth Sisilane, hexamethyldisilane, vinyltrimethoxysilane, γ-mercaptopropylmethyldimethoxysilane, 3-isocyanatopropyltriethoxysilane, 3-acryloxypropyltrimethoxysilane, 3-triethoxylyl-N- (1,3-dimethyl) Silane coupling agents such as rubylidene) propylamine hydrolyzate, isopropyl triisostearoyl titanate, isopropyl tris (dioctylpyrophosphate) titanate, isopropyl tri (N-aminoethyl-aminoethyl) titanate, tetraoctyl bis ( Ditridecyl phosphite) titanate, tetra (2,2-diallyloxymethyl-1-butyl) bis (ditridecyl) phosphite titanate, bis (dioctylpyrophosphate) oxy Siacetate titanate, bis (dioctylpyrophosphate) ethylene titanate, isopropyl trioctanoyl titanate, isopropyl dimethacrylisostearoyl titanate, isopropyl tridodecylbenzenesulfonyl titanate, isopropyl isostearoyl diacryl titanate, isopropyl tri (dioctyl phosphate) titanate, isopropyl tric Examples include titanate coupling agents such as milphenyl titanate and tetraisopropyl bis (dioctyl phosphite) titanate, and these may be used alone or in combination of two or more.
本実施形態の封止樹脂組成物30には、上記の成分以外に、必要に応じて、カーボンブラック等の着色剤;天然ワックス、合成ワックス、高級脂肪酸もしくはその金属塩類、パラフィン、酸化ポリエチレン等の離型剤;シリコーンオイル、シリコーンゴム等の低応力剤;ハイドロタルサイト等のイオン捕捉剤;水酸化アルミニウム等の難燃剤;酸化防止剤等の各種添加剤を配合することができる。 [Others]
In the sealing
以上述べてきた好ましい成分等を適宜使用し、後述する製造方法等で得た本実施形態の封止樹脂組成物のガラス転移温度(つまり硬化させる前の組成物のガラス転移温度)は15℃以上30℃以下が好ましい。前記範囲内とすることで固結しづらく、また金型上ですばやく溶融するという好ましい態様を有することができる。 [Glass transition temperature of encapsulating resin composition]
The glass transition temperature (that is, the glass transition temperature of the composition before curing) of the encapsulating resin composition of the present embodiment obtained by the production method described below using the preferred components described above as appropriate is 15 ° C. or higher. 30 degrees C or less is preferable. By setting it within the above range, it is difficult to consolidate, and it is possible to have a preferable aspect of being quickly melted on a mold.
次に、封止樹脂組成物30の製造方法の一例を説明する。 [Production method]
Next, an example of the manufacturing method of the sealing
内側包装資材20には、直接、封止樹脂組成物30が収容される。内側包装資材20は、例えば、プラスチック袋(例:ポリエチレン袋)、紙袋等の袋であってもよいし、または、所定の強度を有するプラスチック容器、金属容器等であってもよい。内側包装資材20は、例えばポリエチレンで構成されていてもよい。ポリエチレンは、透湿度が5g/m2・日以上20g/m2・日以下のポリエチレンであってもよい。封止樹脂組成物30を収容後、内側包装資材20は封緘される。封緘の手段は特段制限されず、従来のあらゆる手段を利用できる。 <
The encapsulating
外側包装資材10には、封止樹脂組成物30を収容して封緘された内側包装資材20が収容される。また、外側包装資材10内に、直接、封止樹脂組成物30が収容されてもよい。外側包装資材10は、例えば、金属缶や段ボール箱等、所定の強度を有する容器とすることができる。なお、外側包装資材10の使用態様として、複数の外側包装資材10を多段に積み重ねたり、また、外側包装資材10の上に他の物品等を積み重ねたりする場合が考えられる。このような使用態様を想定し、外側包装資材10は、所定の重さ(設計的事項)の物品が積層されても大きく変形せず、当該物品の重さが当該外側包装資材10の内部に収容された封止樹脂組成物30にかからない程度の強度を有するのが好ましい。 <
The
図1に示すように、本実施形態では、封止樹脂組成物30を内側包装資材20に収容し、封緘した後、当該内側包装資材20を外側包装資材10に収容する。そして、封止樹脂組成物30の嵩密度をM(g/cc)、包装資材内に収容された状態における封止樹脂組成物30による堆積物の高さをL(cm)とすると、M×L≦25を満たすようにする。なお、本実施形態において特に0.8g/cc以上1.4g/cc以下、好ましくは0.9g/cc以上1.3g/cc以下の嵩密度の封止樹脂組成物30においてその効果がより顕著となる。本実施形態では、要求性能などにより決定された封止樹脂組成物30の嵩密度Mに基づいて、堆積物の高さL(cm)をコントロールする。具体的には、M×L≦25を満たすように、堆積物の高さL(cm)の上限をコントロールする。高さLは27cm以下、好ましくは25cm以下、より好ましくは22cm以下、より好ましくは15cm以下とする。 <Packing method>
As shown in FIG. 1, in this embodiment, after the sealing
図1に示した実施形態では、1つの外側包装資材10に1つの内側包装資材20を収容していた。しかし、1つの外側包装資材10に複数の内側包装資材20を収容することもできる。 <Modification 1>
In the embodiment shown in FIG. 1, one
図1に示した例及び変形例1では、通常の慣習に従い外側包装資材10の所定の面を底面として地面に載置した状態における高さ(L、HまたはN)を調整(変更)することで、自重力の最大値を所望の範囲に制限する構成を説明した。しかし、保管スペースなどの制限により、通常の慣習に従わず、外側包装資材10のその他の面を底面として地面に載置する使用形態も考えられる。 <Modification 2>
In the example shown in FIG. 1 and the modified example 1, the height (L, H, or N) in a state where the predetermined surface of the
図1に示した実施形態及び変形例1及び2では、封止樹脂組成物30を内側包装資材20に収容し、当該内側包装資材20を外側包装資材10に収容していた。本変形例では、外側包装資材10に直接封止樹脂組成物30を梱包する。その他の構成は、図1に示した実施形態及び変形例1及び2と同様である。 <Modification 3>
In the embodiment and the modifications 1 and 2 shown in FIG. 1, the sealing
本発明者は封止用エポキシ樹脂粒子同士の互着防止について鋭意検討し、温度変調示差走査熱量計を用いて測定したエポキシ樹脂組成物(封止用エポキシ樹脂組成物)の粉粒体ガラス転移温度という尺度が、上述した条件1及び条件2を満たすための設計指針として有効であることをさらに見出した。以下、本実施形態について説明する。 << Second Embodiment >>
The present inventor has intensively studied the prevention of mutual adhesion of epoxy resin particles for sealing, and the powder glass transition of an epoxy resin composition (epoxy resin composition for sealing) measured using a temperature-modulated differential scanning calorimeter. It was further found that the scale of temperature is effective as a design guideline for satisfying the conditions 1 and 2 described above. Hereinafter, this embodiment will be described.
本実施形態の封止樹脂組成物30は、(a)エポキシ樹脂と(b)硬化剤と、(c)無機フィラーとを必須成分として含むが、(d)硬化促進剤、(e)カップリング剤をさらに含んでいてもよい。以下、各成分について具体的に説明する。 <Sealing
The sealing
(a)エポキシ樹脂は、配合割合を除くその他の構成は、第1の実施形態と同様とすることができる。 [(A) Epoxy resin]
(A) An epoxy resin can be made the same as in the first embodiment, except for the blending ratio.
(b)硬化剤は、配合割合を除くその他の構成は、第1の実施形態と同様とすることができる。 [(B) Curing agent]
(B) The configuration of the curing agent other than the blending ratio can be the same as in the first embodiment.
(c)無機フィラーは、含有割合を除くその他の構成は、第1の実施形態と同様とすることができる。 [(C) Inorganic filler]
(C) The inorganic filler can be configured in the same manner as in the first embodiment except for the content ratio.
(d)硬化促進剤の構成は第1の実施形態と同様とすることができる。 [(D) Curing accelerator]
(D) The composition of the curing accelerator can be the same as that of the first embodiment.
(e)カップリング剤の構成は第1の実施形態と同様とすることができる。 [(E) Coupling agent]
(E) The configuration of the coupling agent can be the same as in the first embodiment.
本実施形態の封止樹脂組成物30には、上記の成分以外に、必要に応じて、カーボンブラック等の着色剤;天然ワックス、合成ワックス、高級脂肪酸もしくはその金属塩類、パラフィン、酸化ポリエチレン等の離型剤;シリコーンオイル、シリコーンゴム等の低応力剤;ハイドロタルサイト等のイオン捕捉剤;水酸化アルミニウム等の難燃剤;酸化防止剤等の各種添加剤を配合することができる。 [Others]
In the sealing
(エポキシ樹脂)
エポキシ樹脂1:ビフェニレン骨格含有フェノールアラルキル型エポキシ樹脂(日本化薬(株)製NC3000)
エポキシ樹脂2:ビフェニル型エポキシ樹脂(ジャパンエポキシレジン(株)製、YX4000H) It shows below about the component used by the Example and the comparative example.
(Epoxy resin)
Epoxy resin 1: Biphenylene skeleton-containing phenol aralkyl epoxy resin (NC3000 manufactured by Nippon Kayaku Co., Ltd.)
Epoxy resin 2: biphenyl type epoxy resin (manufactured by Japan Epoxy Resin Co., Ltd., YX4000H)
フェノール樹脂1:ビフェニレン骨格含有フェノールアラルキル樹脂(明和化成(株)製、MEH-7851SS)
フェノール樹脂2:フェニレン骨格含有フェノールアラルキル樹脂(三井化学(株)製、XLC-4L) (Phenolic resin)
Phenol resin 1: Biphenylene skeleton-containing phenol aralkyl resin (Maywa Kasei Co., Ltd., MEH-7851SS)
Phenol resin 2: Phenol aralkyl resin containing phenylene skeleton (Mitsui Chemicals, XLC-4L)
球状無機フィラー1:球状溶融シリカ(平均粒径16μm、比表面積2.1m2/g)
球状無機フィラー2:球状溶融シリカ(平均粒径10μm、比表面積4.7m2/g)
球状無機フィラー3:球状溶融シリカ(平均粒径32μm、比表面積1.5m2/g) (Inorganic filler)
Spherical inorganic filler 1: spherical fused silica (average particle size 16 μm, specific surface area 2.1 m 2 / g)
Spherical inorganic filler 2: Spherical fused silica (
Spherical inorganic filler 3: spherical fused silica (average particle size 32 μm, specific surface area 1.5 m 2 / g)
微球無機フィラー2:球状溶融シリカ(平均粒径1.5μm、比表面積4.0m2/g) Fine spherical inorganic filler 1: spherical fused silica (average particle size 0.5 μm, specific surface area 6.1 m 2 / g)
Fine spherical inorganic filler 2: spherical fused silica (average particle size 1.5 μm, specific surface area 4.0 m 2 / g)
硬化促進剤1:トリフェニルホスフィン
カップリング剤:γ-グリシドキシプロピルトリメトキシシラン
カーボンブラック
ワックス:カルナバワックス (Other ingredients)
Curing accelerator 1: Triphenylphosphine coupling agent: γ-glycidoxypropyltrimethoxysilane carbon black wax: carnauba wax
表2で示す配合のエポキシ樹脂組成物の原材料をスーパーミキサーにより5分間粉砕混合したのち、この混合原料を直径65mmのシリンダー内径を持つ同方向回転二軸押出機にてスクリュー回転数30RPM、100℃の樹脂温度で溶融混練し、冷却、粉砕工程を経て粉砕物としたものを、篩を用いて粒度調整を行い粉粒状の封止樹脂組成物30を得た。封止樹脂組成物30の性状は表2に示す。 <Examples 1, 2, 5>
After the raw materials of the epoxy resin composition having the composition shown in Table 2 were pulverized and mixed for 5 minutes by a super mixer, this mixed raw material was screw rotated at 30 RPM at 100 ° C. in a co-rotating twin screw extruder having a cylinder inner diameter of 65 mm. A powdered encapsulating
実施例1と同様に封止樹脂組成物30を得た。封止樹脂組成物30の性状は表2に示す。 <Examples 3 and 4>
A sealing
表2に示す配合で実施例1と同様に封止樹脂組成物を得た。 <Comparative Examples 1 to 5>
A sealing resin composition was obtained in the same manner as in Example 1 with the formulation shown in Table 2.
実施例及び比較例における粉粒状の封止樹脂組成物を下記の方法で調整、評価した。 <Evaluation method>
The granular sealing resin compositions in Examples and Comparative Examples were adjusted and evaluated by the following methods.
(株)マウンテック製MACSORB HM-MODEL-1201を使用し、BET流動法により評価した。 1. Specific surface area (SSA)
MACSORB HM-MODEL-1201 manufactured by Mountec Co., Ltd. was used and evaluated by the BET flow method.
(株)島津製作所製、SALD-7000を使用し、レーザー回折式粒度分布測定法にて評価した。D50はメジアン径である。 2. Average particle size of inorganic filler (D 50 )
SALD-7000 manufactured by Shimadzu Corporation was used and evaluated by a laser diffraction particle size distribution measurement method. D 50 is the median diameter.
ロータップ振動機に備え付けた目開き2.00mm、1.00mm、及び0.106mmのJIS標準篩を用いて粒度分布を調整、決定した。 3. Particle size distribution of encapsulating resin composition granules The particle size distribution was adjusted and determined using JIS standard sieves with mesh openings of 2.00 mm, 1.00 mm, and 0.106 mm provided in a low tap vibrator.
得られた封止樹脂組成物を一旦所定の寸法のタブレットに打錠し、トランスファー成形機を用い、金型温度175±5℃、注入圧力7MPa、硬化時間120秒で、直径50mm×厚さ3mmの円盤を成形し、質量、体積を求め硬化物比重を計算した。 4). True specific gravity The obtained sealing resin composition is once compressed into tablets of a predetermined size, using a transfer molding machine, with a mold temperature of 175 ± 5 ° C., an injection pressure of 7 MPa, a curing time of 120 seconds, a diameter of 50 mm × thickness A disk with a thickness of 3 mm was molded, and the mass and volume were determined to calculate the specific gravity of the cured product.
パウダーテスター(ホソカワミクロン株式会社製)を用い、内径50.46mm、深さ50mm、容積100cm3の測定容器の上部に円筒を取り付けたものに封止樹脂組成物の試料をゆるやかに入れた後、180回のタッピングを行い、その後、上部円筒を取り除き、測定容器上部に堆積した試料をブレードですりきり、測定容器に充填された試料の重量を測定することにより求めた。 5. Bulk density After using a powder tester (manufactured by Hosokawa Micron Co., Ltd.) and gently putting a sample of the sealing resin composition on a measuring vessel having an inner diameter of 50.46 mm, a depth of 50 mm, and a volume of 100 cm 3 attached to a cylinder. Then, tapping was performed 180 times, and then the upper cylinder was removed, the sample deposited on the upper part of the measurement container was ground with a blade, and the weight of the sample filled in the measurement container was measured.
低圧トランスファー成形機(コータキ精機社製、「KTS-15」)を用いて、ANSI/ASTM D 3123-72に準じたスパイラルフロー測定用金型に、175℃、注入圧力6.9MPa、保圧時間120秒の条件で、各実施例および各比較例の封止樹脂組成物を注入し、流動長を測定し、これをスパイラルフロー(cm)とした。 6). Spiral Flow Using a low-pressure transfer molding machine (“KTS-15”, manufactured by Kotaki Seiki Co., Ltd.), a spiral flow measurement mold conforming to ANSI / ASTM D 3123-72 was maintained at 175 ° C., injection pressure 6.9 MPa. Under the conditions of a pressure time of 120 seconds, the sealing resin compositions of the respective examples and the comparative examples were injected, and the flow length was measured, which was defined as a spiral flow (cm).
図9に示したとおり、パウダーテスター(ホソカワミクロン(株)製、型式―PT-E)に備え付けた直径80mmの円板状水平板205の中心に向けて、漏斗201を用いて垂直方向から常温戻し処理後の顆粒状の樹脂組成物202を投入し、水平板205上に円錐状の顆粒体204を形成させた。顆粒状の樹脂組成物202の投入は円錐が一定形状を保つまで行い、分度器を用いて図5のように仰角(φ)を求め安息角とした。次に、水平板205と同じ台座206上にある109gの分銅203を高さ160mmのところから三回落下させ、衝撃によって一部の顆粒状の樹脂組成物が崩壊して脱落した後、水平板205上に残った円錐状の顆粒体207の仰角(θ)を、分度器を用いて図5のように求め崩壊角とした。そして、測定した安息角と崩壊角との差を求め差角とした。 7. Difference angle As shown in FIG. 9, from the vertical direction using a
常温戻し処理後の顆粒状の樹脂組成物をロータップ振動機に備え付けた目開き2mmのJIS標準篩を用い、20分間に亘って振動させながら40gの試料を篩に通して分級し篩に残る粒状体や粒体の重量を計測した。このように計測した重量を分級前の試料の重量を基準にして重量比を算出した。 8). Content of sieve pass product with 2 mm opening Use a JIS standard sieve with 2 mm opening provided with a low-tap vibrator with the granular resin composition after returning to room temperature, and shake 40 g of sample over 20 minutes. The particles were classified by passing through a sieve, and the weight of granules and granules remaining on the sieve was measured. The weight ratio was calculated based on the weight thus measured based on the weight of the sample before classification.
温度変調示差走査熱量計(以下モジュレイテッドDSCまたはMDSCと記載する)を使用し、本発明の封止樹脂組成物(硬化前のもの)を5℃/min、大気下で測定し、JIS K7121に従って値を求めた。 9. Sealing resin composition glass transition temperature (Tg) by MDSC
Using a temperature-modulated differential scanning calorimeter (hereinafter referred to as “modulated DSC or MDSC”), the sealing resin composition of the present invention (before curing) is measured at 5 ° C./min in the atmosphere, according to JIS K7121 The value was determined.
厚み0.5mm、幅50mm、長さ210mmの回路基板上に、厚み0.3mm、7.5mm角の半導体素子を銀ペーストにて接着し、径18μm、長さ7mmの金線ワイヤーをピッチ間隔60μmで半導体素子と回路基板に接合したものを、圧縮成形機(TOWA株式会社製、PMC1040)により一括で封止成形し、MAP成形品を得た。この際の成形条件は、金型温度175℃、成形圧力3.9MPa、硬化時間120秒で行った。次いで、得られたMAP成形品をダイシングにより個片化し、模擬半導体装置を得た。得られた模擬半導体装置におけるワイヤー流れ量を、軟X線装置(ソフテックス株式会社製、PRO-TEST-100)を用いてパッケージの対角線上にある最も長い金ワイヤー4本(長さ7mm)の平均の流れ率を測定し、ワイヤー流れ率(ワイヤー流れ量/ワイヤー長×100(%))を算出した。 10. Wire deformation On a circuit board with a thickness of 0.5 mm, a width of 50 mm, and a length of 210 mm, a semiconductor element with a thickness of 0.3 mm and a 7.5 mm square is adhered with a silver paste, and a gold wire having a diameter of 18 μm and a length of 7 mm is formed. What was joined to the semiconductor element and the circuit board with a pitch interval of 60 μm was collectively encapsulated with a compression molding machine (PMC1040, manufactured by TOWA Corporation) to obtain a MAP molded product. The molding conditions at this time were a mold temperature of 175 ° C., a molding pressure of 3.9 MPa, and a curing time of 120 seconds. Next, the obtained MAP molded product was separated into pieces by dicing to obtain a simulated semiconductor device. Using the soft X-ray device (PRO-TEST-100, manufactured by Softex Co., Ltd.), the wire flow rate in the obtained simulated semiconductor device was measured for the four longest gold wires (
Claims (15)
- 顆粒状の封止樹脂組成物を包装資材に収容し、かつ、10℃以下の状態で運搬する前記顆粒状の封止樹脂組成物の運搬方法であって、
前記封止樹脂組成物の嵩密度をM(g/cc)、
前記包装資材内に収容された状態における、前記封止樹脂組成物による堆積物の高さをL(cm)とすると、M×L≦25を満たし、
前記封止樹脂組成物を収容した前記包装資材を、温度4℃、相対湿度35%で24時間放置し、次いで、温度23℃、相対湿度50%で24時間放置した後に前記包装資材から取出した前記封止樹脂組成物は、差角が10度以上となる運搬方法。 The granular sealing resin composition is contained in a packaging material, and the granular sealing resin composition is transported in a state of 10 ° C or less,
The bulk density of the sealing resin composition is M (g / cc),
When the height of the deposit by the sealing resin composition in a state accommodated in the packaging material is L (cm), M × L ≦ 25 is satisfied,
The packaging material containing the sealing resin composition was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours, and then taken out from the packaging material. The encapsulating resin composition is a transport method in which the difference angle is 10 degrees or more. - 顆粒状の封止樹脂組成物を包装資材に収容し、かつ、10℃以下の状態で運搬する前記顆粒状の封止樹脂組成物の運搬方法であって、
前記封止樹脂組成物の嵩密度をM(g/cc)、
前記包装資材内に収容された状態における、前記封止樹脂組成物による堆積物の高さをL(cm)とすると、M×L≦25を満たし、
前記封止樹脂組成物を収容した前記包装資材を、温度4℃、相対湿度35%で24時間放置し、次いで、温度23℃、相対湿度50%で24時間放置した後に前記包装資材から取出した前記封止樹脂組成物は、目開き2mmの篩パス品の含有率が90重量%以上となる運搬方法。 The granular sealing resin composition is contained in a packaging material, and the granular sealing resin composition is transported in a state of 10 ° C or less,
The bulk density of the sealing resin composition is M (g / cc),
When the height of the deposit by the sealing resin composition in a state accommodated in the packaging material is L (cm), M × L ≦ 25 is satisfied,
The packaging material containing the sealing resin composition was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours, and then taken out from the packaging material. The sealing resin composition is a transportation method in which the content of a sieve pass product having an opening of 2 mm is 90% by weight or more. - 請求項1又は2に記載の運搬方法において、
前記包装資材は、前記封止樹脂組成物が直接収容される内側包装資材と、前記内側包装資材が収容される1つまたは複数の部屋を内部に有する外側包装資材とを含み、
前記外側包装資材内に収容された状態における1つの前記内側包装資材の高さをH(cm)とすると、M×H≦25を満たす運搬方法。 In the transportation method according to claim 1 or 2,
The packaging material includes an inner packaging material in which the sealing resin composition is directly accommodated, and an outer packaging material having one or more rooms in which the inner packaging material is accommodated,
A transport method that satisfies M × H ≦ 25, where H (cm) is the height of one inner packaging material in a state of being accommodated in the outer packaging material. - 請求項1又は2に記載の運搬方法において、
前記包装資材は、前記封止樹脂組成物が直接収容される1つまたは複数の部屋を内部に有する外側包装資材を含み、
前記外側包装資材の底面を地面に載置した状態における前記部屋の高さをN(cm)とすると、M×N≦25を満たす運搬方法。 In the transportation method according to claim 1 or 2,
The packaging material includes an outer packaging material having one or more rooms in which the sealing resin composition is directly accommodated,
A transport method that satisfies M × N ≦ 25, where N (cm) is the height of the room when the bottom surface of the outer packaging material is placed on the ground. - 請求項1から4のいずれか1項に記載の運搬方法において、
前記封止樹脂組成物は、無機フィラーを含む運搬方法。 In the conveyance method of any one of Claim 1 to 4,
The sealing resin composition is a transportation method including an inorganic filler. - 請求項1から5のいずれか1項に記載の運搬方法において、
前記封止樹脂組成物は、エポキシ樹脂を含む運搬方法。 In the conveyance method of any one of Claim 1 to 5,
The sealing resin composition is a transportation method including an epoxy resin. - 請求項1から6のいずれか1項に記載の運搬方法において、
前記封止樹脂組成物は、フェノール樹脂を含む運搬方法。 In the conveyance method of any one of Claim 1 to 6,
The said sealing resin composition is a conveying method containing a phenol resin. - 請求項1から4のいずれか1項に記載の運搬方法において、
前記封止樹脂組成物は、圧縮成形により素子を封止するために用いられる顆粒状の封止用エポキシ樹脂組成物であって、
(a)エポキシ樹脂と、(b)硬化剤と、(c)無機フィラーとを必須成分として含み、
温度変調示差走査熱量計を用いて測定した前記封止用エポキシ樹脂組成物の粉粒体ガラス転移温度が12℃以上35℃以下である運搬方法。 In the conveyance method of any one of Claim 1 to 4,
The sealing resin composition is a granular sealing epoxy resin composition used for sealing an element by compression molding,
Including (a) an epoxy resin, (b) a curing agent, and (c) an inorganic filler as essential components,
The conveyance method whose powder particle glass transition temperature of the said epoxy resin composition for sealing measured using the temperature modulation differential scanning calorimeter is 12 degreeC or more and 35 degrees C or less. - 請求項1から8のいずれか1項に記載の運搬方法において、
前記封止樹脂組成物は、ビフェニルアラルキル樹脂を含む運搬方法。 In the conveyance method of any one of Claim 1 to 8,
The encapsulating resin composition includes a biphenyl aralkyl resin. - 請求項1から9のいずれか1項に記載の運搬方法において、
前記封止樹脂組成物は、ビフェニル型エポキシ樹脂を含む運搬方法。 In the conveyance method of any one of Claim 1 to 9,
The encapsulating resin composition includes a biphenyl type epoxy resin. - 請求項1から10のいずれか1項に記載の運搬方法において、
前記封止樹脂組成物は、ホスフィン化合物とキノン化合物との付加物を含む運搬方法。 The transportation method according to any one of claims 1 to 10,
The sealing resin composition is a transportation method including an adduct of a phosphine compound and a quinone compound. - 請求項1から11のいずれか1項に記載の運搬方法において、
前記封止樹脂組成物が直接収容される前記包装資材は、ポリエチレンで構成されている運搬方法。 The transportation method according to any one of claims 1 to 11,
The said packaging material in which the said sealing resin composition is directly accommodated is the conveyance method comprised with polyethylene. - 請求項12に記載の運搬方法において、
前記ポリエチレンは、透湿度が5g/m2・日以上20g/m2・日以下である運搬方法。 The transport method according to claim 12,
The polyethylene has a moisture permeability of 5 g / m 2 · day to 20 g / m 2 · day. - 包装資材と、
前記包装資材内に収容された顆粒状の封止樹脂組成物と、
を有し、
前記封止樹脂組成物を収容した前記包装資材を、温度4℃、相対湿度35%で24時間放置し、次いで、温度23℃、相対湿度50%で24時間放置した後に前記包装資材から取出した前記封止樹脂組成物は、差角が10度以上である梱包物。 Packaging materials,
A granular sealing resin composition housed in the packaging material;
Have
The packaging material containing the sealing resin composition was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours, and then taken out from the packaging material. The sealing resin composition is a package having a difference angle of 10 degrees or more. - 包装資材と、
前記包装資材内に収容された顆粒状の封止樹脂組成物と、
を有し、
前記封止樹脂組成物を収容した前記包装資材を、温度4℃、相対湿度35%で24時間放置し、次いで、温度23℃、相対湿度50%で24時間放置した後に前記包装資材から取出した前記封止樹脂組成物は、目開き2mmの篩パス品の含有率が90重量%以上である梱包物。 Packaging materials,
A granular sealing resin composition housed in the packaging material;
Have
The packaging material containing the sealing resin composition was left at a temperature of 4 ° C. and a relative humidity of 35% for 24 hours, and then left at a temperature of 23 ° C. and a relative humidity of 50% for 24 hours, and then taken out from the packaging material. The sealing resin composition is a packaged product having a sieve pass product having a mesh opening size of 2 mm and a content of 90% by weight or more.
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JP2001151856A (en) * | 1999-11-30 | 2001-06-05 | Dainippon Ink & Chem Inc | Epoxy resin composition for sealing electronic part |
JP2001234196A (en) * | 1999-12-14 | 2001-08-28 | Lion Corp | Granular detergent composition and granular detergent composition filled in transparent container |
JP2004090971A (en) * | 2002-08-30 | 2004-03-25 | Hitachi Chem Co Ltd | Packaging method for epoxide resin molding material for sealing semiconductor |
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KR20160029070A (en) | 2016-03-14 |
CN105358452B (en) | 2017-05-17 |
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