Adhesives and Epoxies Q&A
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I have an application in which opaque parts bond with a Super Glue-type cyanoacrylate. There is much surface area and I have a very good bond. Will gamma sterilization affect my bond strength?Most cyanoacrylates will survive 1×, 2×, and sometimes even 3× gamma sterilization without a significant impact on bond strength. However, repeated gamma sterilization will add additional cross-linking, which will start to reduce elongation. As most cyanoacrylates are already brittle materials (depending on the grade), the adhesive may become even more brittle. Drop tests, impact testing, or tensile testing may be a good indicator of the final impact on your bond strength.
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Are methanol, ethanol, acetone, or acetonitrile FDA approved?Methanol, ethanol, acetone, or acetonitrile are generally not FDA approved. These solvents bond plastics together by melting them and allowing them to intermingle. As the solvent evaporates, the plastics harden to form a strong weld. The choice of which grade of solvent to use is up to the medical device manufacturer. Higher-purity grades are more expensive than lower-purity grades. Since the solvent evaporates and does not remain in the bond line, it is not normally tested for biocompatibility.
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Is there a temporary adhesive to bond glass and withstand a temperature of 1400°F?Before this question can be answered, we need to ask how you define “temporary.” Only some materials will withstand temperatures up to 1400°F. Companies such as Cotronics Corp. (Brooklyn, NY) and Aremco (Valley Cottage, NY)—to name just a few—offer high-temperature adhesives. These adhesives are often modified with fillers such as alumina, zircon, mica, or ceramics that allow the adhesive to withstand higher-temperature environments. Some materials, including liquid materials or tape-type products, have a continuous-service temperature of 1500°F and a melting point of 2800°F. So in one sense, these adhesives are permanent at 1500°F but temporary as you raise the temperature. Some epoxy systems can withstand temperatures up to 4000° and 5000°F.
Thus, the question becomes: How long should the adhesive survive at 1400°F? If the answer is minutes, finding a material that can survive short bursts of high temperatures for only a little while may be sufficient. For this purpose, a number of different chemistries, such as silicone or epoxy, are available. Typically, unfilled organic adhesives such as acrylics and urethanes will break down long before they reach 1400°F.
The last question is: What are the properties needed? Does the adhesive need to be clear, or is opaque acceptable? How do you want to remove the material? Unfortunately, there is no simple answer to these questions. The technical support groups at the companies mentioned above may be able to help further or recommend options for you to consider.
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I need to bond acrylonitrile butadiene styrene (ABS) to ABS in a pure-water environment (50° to 180°F). But the concern about leaching chemicals into the pure water is high. What FDA-approved solvent choices do I have?An information sheet from Ineos Nova lists various solvents such as cyclohexanone, cyclohexanone/tetrahydrofuran, cyclohexanone with various medical-grade acrylic polymers dissolved in the solvent for added strength, and various other combinations.
Solvent grades are typically not listed as medical grade or FDA approved but rather by the purity level of the solvent. Obtaining the solvent of choice with the highest purity (99.9% or higher) would limit the potential of leaching chemicals into the water. Sigma Aldrich or Alpha Aesar both provide small quantities of these solvents in various grades for evaluation purposes. Methyl ethyl ketone is an alternative solvent system. However, because of their odor, flammability, and explosive-material storage requirements, using solvents requires special handling and is carefully monitored by the EPA. Dispensing systems such as those offered by Tecnoideal are options to limit operator exposure.
If you want to consider a solvent-free adhesive, looking at a one-part light-curable adhesive such as Dymax’s 1161-M is possible if you can get visible light to the bond line (the nonopaque parts). Alternatively, a two-part urethane or epoxy from companies such as Epoxy Technology or 3M (to name two options) can be considered. These alternatives can provide a bond almost as strong as that provided by a solvent and with fill gaps in the molded ABS bond lines. In addition, they are much more environmentally friendly.
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Our research lab is looking for a medical-grade adhesive for two applications: bonding Dacron cloth to silver plate and bonding glass and a polymethylmethacrylate (PMMA) optical cylinder in a silver tube. The adhesive must be moisture resistant and should last for a long time (20 years). Please suggest a product.Dacron is a commercial name for polyethylene terephthalate (PET). Bonding cloth to a rigid substrate such as silver plate can be done in a few different ways. Bonding to cloth is mostly a mechanical lock that forms by encapsulating strands of the cloth and then locking them to the rigid substrate. The viscosity of the adhesive will play a role, since the thinner the viscosity, the more it will wick into the cloth. A very-high-viscosity adhesive will not wick very far into the cloth. A two-part epoxy such as that offered by Loctite or 3M and a two-part urethane such as that offered by Lord Corp. are two avenues to explore. A silicone adhesive, offered by such companies as Dow Corning, Momentive Performance Materials, NuSil Technology, or other silicone manufacturers, may also do the trick.
Bonding glass and PMMA may also work with the same adhesive you use to bond Dacron cloth to silver plate, but depending on the gap between the parts and method of assembly, it may require a lower-viscosity material. The epoxy and silicone systems will be moisture resistant and have good usage life, but most manufacturers will not warrantee an adhesive for 20 years. If the bond area can be subjected to light, one-part light-curable urethane acrylates such as 203A-CTH or 209-CTH from Dymax are options.
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I am using some ultraviolet curing adhesives and was told that there is a risk of leaving uncured monomers in the adhesive. I have heard that they could cause adhesive failure over the long term (such as 6 months or more), where the monomers dissolve or soften the cured resin. Assuming my cured adhesive is very hard and tests well for tensile strength, is it true that uncured monomers (in very small amounts) can cause the adhesive bond to weaken over time?If a material is fully cured, there is no risk of resolvating the adhesive because of uncured monomers left behind, since everything that could react has been reacted. However, it is our experience that the light-curing adhesives used by many people do not actually reach a fully cured state. Instead of reaching a fully cured state in which 96 to 100% of reactable materials have been converted, a particular process or part configuration will sometimes reach only 75 to 80% conversion. If a material reaches only a semicured state, it could appear to be cured, providing good tensile strength and a cured surface, but have unreacted monomers at some level within the adhesive. These unreacted monomers can then resolvate or attack the surrounding adhesive, thereby weakening it and the bond joint.
This problem will be noticeable with accelerated aging, or within one to six months. A good qualification process will eliminate this risk. There are several qualification options:
● Evaluate various safety factors (cure times or intensity at 1.3×, 1.5×, 2.0×, 3.0×) to verify that the adhesive strength and properties have reached a plateau.
● Run accelerated aging tests at a moderate temperature to verify long-term stability and evaluate the adhesive in a process using Fourier transform infrared spectrometry to identify the presence of uncured monomers. A skilled analytical chemist can identify a double-bond peak, indicating the presence of uncured adhesive, or the lack of a double-bond peak, indicating that all reactable materials have been reacted.
● Use photodifferential scanning calorimetry to measure the change in crosslink density.
Building a process to ensure that you reach a fully cured state and have a good safety margin is the key to successfully using a light-curable adhesive.
“See-Cure Adhesive Technology,” available from Dymax, has a color indicator that changes from blue to clear when full cure has been reached. This tool helps users to identify when the adhesive has reached a fully cured state.
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I am trying to understand the UV curing process. A question comes to mind about how I can decide that the adhesive is fully cured. What are the critical parameters that I need to control in order to gain good consistency for curing? Also, I tried to cure some adhesive on a piece of stainless-steel coupon. A small drop of adhesive was placed on the coupon, forming a kind of round-shaped droplet. I wonder whether the curing is more efficient on the surface of the droplet or on the inside of the droplet.Very good question! Light-curing adhesives—whether they are cured using ultraviolet (UV) light, visible light, or a combination of UV and visible light—cure from the surface closest to the lamp. If you have a droplet, the surface will cure first, and then the rest of the dome will follow. The last area to cure is against the substrate, so this leads to the question: How do you know when the adhesive is fully cured?
Adhesion to the substrate is one way to evaluate full cure. A simple test is to use a tool to get underneath the droplet. If there is liquid at the interface, then the adhesive is not fully cured. In such cases, you would need to increase either the intensity of the lamp or the exposure time. Most applications require a minimum amount of energy to achieve a good cure. Energy, or Joules/cm2, is arrived at by multiplying intensity (watts/cm2) by dose (seconds). Since you want to build a process around the total amount of Joules needed to reach full cure, you can vary either the intensity or the time needed for curing. And as long as you reach the minimum energy for a given lamp, you should have a robust process.
The best way to determine whether you have a robust process is to run adhesion strength tests by bonding laps or components together to see when full or maximum strength is achieved or to perform physical characterizations for such parameters as durometer, elongation, tensile, or modulus under different conditions. When full strength is reached, additional energy (intensity or time) does not lead to an increase in adhesion properties. Compare the results of your process to the specifications in your manufacturer’s data sheet. The data sheet may indicate that the material will ultimately reach a specific durometer, such as A-40, D-60, or D-90. For example, under most conditions, if you were plotting durometer/hardness, the hardness will build (incomplete cure) and then plateau (complete cure). You should also build in enough time to add a safety margin, and then you will achieve a robust process. It is important to have a radiometer at hand because this device will tell you the energy intensity in watts/cm2 or milliwatts/cm2, which will be critical to the application.
The ability to cure on the surface can be affected by a phenomenon called oxygen inhibition. Some older adhesive technologies may be affected by oxygen during the cure process, which leaves a slightly tacky residue on the surface. The best way to overcome this issue is to start with a higher intensity, which allows you to cure the adhesive for a shorter period of time. New materials are being designed to overcome this issue, but lamp selection and bulb spectrum are important when developing a new process.
Dymax has a new technology to help you define the parameters of a robust process and ensure that the material will cure fully during production. See Cure Technology is a patent-pending adhesive method available in many Dymax products that allows the adhesive to appear bright blue in its uncured state. Upon reaching full cure under a light source, the blue color disappears, leaving a colorless clear adhesive in the bond line. The adhesive becomes clear only when it has reached enough energy to be fully cured. This product was designed to incorporate a safety margin before the color change happens, so it is an effective way not only to build a process but also to have a quality inspection system within the adhesive to tell you if you have reached full cure.
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We currently use a light-curing acrylated urethane adhesive to bond PVC tubing to a part molded from TPE, but we are seeing the adhesive turn yellow and tacky after gamma sterilization and accelerated aging. The PVC tubing is also becoming harder in the bond area. These characteristics are conspiring to cause bond failure. The suspect is di(2-ethylhexyl)phthalate plasticizer (DEHP) leaching out of the PVC and entering the adhesive. In your opinion, is this the likely cause? Once cured, I would have expected the adhesive to be impervious to DEHP.I agree that the suspect is the plasticizer migrating during the sterilization and accelerated aging process. Plasticizers such as DEHP and butyl octyl phthalate (BOP) often migrate with heat and time from areas of high concentration to areas of low concentration. It does not matter if the adhesive is cured or uncured. Plasticizers in effect solvate the adhesive and migrate into it, often causing it to change color and become gummy or tacky. Just as plasticizers keep PVC nice and flexible in the cured state, they migrate away from the PVC under the right conditions.
In this case, the plasticizer migrated into the adhesive, eventually leading to bond failures. This result can be tested by subjecting the PVC tubing alone to the same heating and accelerated aging conditions and wiping the surface periodically throughout the process. Testing the wipe media for contaminants such as DEHP or BOP can indicate the process step that causes this migration and how much contaminant is migrating. Instead of wiping, you can also “chemically wash” the part with a proper solvent, collect the solvent, and analyze it using gas chromatography.
To fix the problem, we would recommend that you try different PVC tubing with a less mobile plasticizer, or switch to comparable polyurethane tubing that has physical properties similar to those of PVC but does not require a plasticizer. Changing the chemistry of the adhesive, while possible, is a last resort in most cases.
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Do you know of a product such as silicone that is used to make molds with a relative density of 1?There are a number of silicone mold-making materials available from silicone-manufacturing companies. Products from Wacker, Rhodia, NuSil, Momentive, and Dow Corning all have a typical relative density of 1.06 to 1.15 g/cm3. While Dow Corning has a nice Mold Making Solutions Web page, product selection may best be achieved by contacting a distributor in your area that carries these products. They are set up to answer questions quickly and serve as a conduit to the larger companies.
Urethane rubbers can also be used for mold making. During a quick search, I found a urethane rubber product, PMC-121, from Smooth-On Liquid Rubber, that has a relative density of 1.04 g/cm3. There are many urethane materials for mold making, so the choice is yours to pick a vendor that specializes in the mold-making materials that suit your needs.
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To ensure reproducibility of the product and to be able to vary the physical properties of the resulting molecular composition of the resulting polymer chains, how can one control the soft-segment and hard-segment positional composition of a finished polymer when one has a diisocyanate plus two or more polyols with different molecular weights? I want to achieve an acrylic emulsion technology to create various copolymers with feed rates and feed composition similar to those of monomers.Adjusting the feed rates, order of addition, and feed composition will help create a block copolymer–type system with blocks of soft and hard segments. The chain lengths of the polymers will dictate the length of the blocks, but in a straight blending-type reaction vessel, how the blocks form together will still be random.
You can get AAABBBAAABABABAABAAABAABBBBBAAABBA—a random sequence that will form if you are not careful. A step-growth block copolymer system can help form a repeatable and controlled AABBAABBAABBAABB structure. Vendors of the various polyols may have ideas on how to assemble a stepwise growth structure.



