Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – From phenol – phenol ether – or inorganic phenolate
Reexamination Certificate
1999-01-22
2001-10-02
Sellers, Robert E. L. (Department: 1712)
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
From phenol, phenol ether, or inorganic phenolate
C523S456000, C523S466000, C523S467000, C525S107000, C525S523000, C528S092000
Reexamination Certificate
active
06297344
ABSTRACT:
BACKGROUND OF THE INVENTION
The invention relates to a casting resin system with improved storage characteristics, The casting resin system is suitable for the formation of glued bonds with dimensional tolerances in the micrometer and sub-micrometer (“&mgr;m and sub-&mgr;m”) region (smaller than 1 &mgr;m)
From Assignee internal patent application docket number 94 E 1887 (official file number not yet known), whose content is hereby incorporated by reference, a thermally hardenable single-component adhesive system is known that achieves an increase in viscosity in long-term storage, i.e. for example, storage of six months or longer. An increase in viscosity leads to modified runoff and flow characteristics of the adhesive system, which make dosing precision difficult. In particular, in the application of small quantities of adhesive in micro-gluing technology, these effects then often cause problems that make a reproducible adhesive application more difficult for mass production, e.g. in the field of microoptics. For the inhibition of the initiators contained in the mixture, these adhesive systems often have basic additives. In addition, the (often volatile) basic additives can lead during processing to odor annoyances that are harmful to health, and have an adverse effect on the hardening reaction in the gluing, above all in thinner layers.
There is thus a need for adhesive systems in which the basic additives can be omitted, and which have an improved storage stability with respect to the receipt of their low viscosity, i.e. their viscosity remains almost unchanged over the storage period.
SUMMARY OF THE INVENTION
It is thus all object of the present invention to provide an adhesive system that can do without basic additives and has improved storage stability with respect to its low viscosity.
The general recognition of the invention is that the addition of small quantities of metal complex compound, advantageously zinc complexes, to the known adhesive systems has the effect that the adhesive systems retain their low viscosity for a considerably longer time during storage in the refrigerator (at approx. 5° C. to 8° C.).
The subject matter of the present invention is a thermally hardenable single-component adhesive system. The adhesive system includes the following components:
60-98% weight percent of a casting resin
2-30 weight percent of an alcohol or a sugar,
0.2-2.0 weight percent of a thermal initiator,
0.2-2.0 weight percent of a bonding agent and/or
0-3.0 weight percent of a flow improver and/or
0-4 weight percent of a thixotropic agent and/or of a flow modifier, and
0.2-5.0 weight percent of a metal complex compound.
In addition, the subject matter of the present invention is the use of the adhesive system for the formation of adhesives with dimensional tolerances in the &mgr;m and sub-&mgr;m region.
DETAILED DESCRIPTION OF THE PRESENTLY PREFERRED EMBODIMENTS
The present invention provides an adhesive system with improved storage stability. The inventors have discovered that the addition of a metal complex compound to known adhesive systems allows for the retention of low viscosity for considerably longer times during storage. As a result, the adhesive system of the present invention can be used unproblematically, even after long periods of storage, for microdosing technology.
Pursuant to the present invention, the adhesive system includes a casting resin, an alcohol or a sugar, a thermal initiator, a bonding agent and a metal complex. In a preferred embodiment, the casting resin is an epoxy casting resin and the alcohol is a multivalent alcohol. Still further, the adhesive of the present invention can also include known additives that thereby provide additional characteristics to the adhesive.
In the present invention, “casting resin” is understood to mean thermally hardenable resin systems and reaction resins that are of such low viscosity that by means of casting they can be brought into a corresponding shape in which they can then be hardened thermally, i.e. by means of temperature increase with the presence of suitable additives i.e., initiators, accelerators, and other components). According to the invention, a preferred casting resin is epoxy casting resin. In the inventive formulation, the casting resin is contained in a quantity of 60-98 weight percent, advantageously in a quantity of 75 to 95 weight percent, preferably between 80 and 95 weight percent, and particularly preferably in the range from 85 to 93 weight percent.
As an“epoxy casting resin,” cycloaliphatic epoxy resins can be used, such as the resin CY177 available from—therefor Ciba Geigy (a bis3,4-epoxycyclohexylmethyl)-adipate or the resin CY179, likewise of available from Ciba Geigy (a 3,4-epoxycyclohexylmethyl-3′, 4′-epoxycyclohexane carboxylate). In addition, linear aliphatic epoxy resins, e.g. epoxied polybutadiene or epoxied soybean oil, are suitable for use in the present invention. Other cationically hardening resins, such as vinyl ether or vinyl aromates, are likewise suitable. In addition, epoxy resins of the glycidylether type are suitable. The following can serve as a basis for the glycidylether: bisphenols (e.g. bisphenol A,) di- or polyhydroxyaromates, (e.g. resorcin,) polyarylalkyls with phenolic OH groups, novolaks, polyalkylene glycols or also multiple alcohols (e.g. butane diol, hexane diol, glycerine or pentaerythritol). In addition, glycidylether ester-type compounds are suitable, (e.g. parahydroxybenzoic acid-glycidylether ester); pure glycidyl ester of multiple carbon acids with aliphatic or aromatic core (e.g. hexahydrophthalic acid or phthalic acid).
According to the invention, alcohols with 1-15 hydroxy groups or sugar are used as“alcohols or sugar.” Preferably, alcohols with 1 to 5 hydroxy groups are used. The skeletal structure of the alcohol or sugar can thereby vary arbitrarily. It can be aliphatic, cyclic or bicyclic. It can consist only of single bonds or also of multiple bonds, and can also be an aromatic system. Among others, the TCD alcohol DM available from of the Hoechst company is preferably used, which is a 3(4),8(9)bis(hydroxymethyl)tricyclo[5.2.1.0
2,6
]decane. The (preferably multivalent) alcohol is contained in the adhesive formulation with a mass portion between 2 and 30 weight percent. It preferably has a mass portion between 2.5 and 20 weight percent, particularly preferably a portion between 4.5 and 12 weight percent.
As a thermal initiator, all standard initiators that harden according to a cationic mechanism, e.g. onium salts, can be used. Here S-benzylthiopheniumhexaflouroantimonate of the Aldrich company, is preferably used.
As a bonding agent, A187 available from the Huls company is used, which is a 3-glycidyloxypropyltrimethoxysilane.
As a flow improver, Modaflow (Monsanto company), which is a copolymer of ethyl acrylate and 2-ethylhexyl acrylate, can be used, and as flow modifiers or thixotropic agents, the commercially available aerosil types of the Degussa company can, for example, be used.
As metal complex compounds, Zn
2+
compounds or other metal complexes of transition metals can preferably be used. Suitable metal compounds for use in the metal complexes include:
zircon, iron, cobalt, titanium, nickel, molybdenum and manganese, or
tin, magnesium or aluminum, as well as
rare earths such as cerium.
“To make the metal complex compounds, such metal compounds are combined” with standard organic ligands, such as amino acids, acetate, general carbonic acids, amines and acetylacetonates, etc. The added quantities of zinc complex compound is between 0.2 and 5 weight percent, preferably less than 3 weight percent. The added quantity is particularly preferably less than 1 weight percent.
Besides the components already stated, further known additives can also be contained in the inventive adhesive system. As a result, the adhesive systems also receive additional characteristics, such as a particular color or transparency, as well as flame retardance or heat resistance. Additives in this sense can thus be, for example, dyes, pig
Bayer Heiner
Hohn Klaus
Schiff & Hardin & Waite
Sellers Robert E. L.
Siemens Aktiengesellschaft
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