Isopropyl Alcohol

Example 2

As discussed herein above, the disclosed methods improve the antiseptic properties of a dental implant without using charged metallic ions via conversion of the nitrogen moieties in titanium nitride surface to a positively charged quaternary ammonium via a Menschutkin reaction.

To prepare the antibacterial quaternized TiN surface, an implant which has been coated with TiN was used. The implant was cleaned to improve yield. The implant was washed with two solvents in sequence, acetone and isopropanol, to remove any dust particulate and other residue. The native oxide layer was removed by sonicating in 1:10 HCl:deionized water for 1 minute. This treatment additionally removes any residue that may not have been removed by the solvents. Acetonitrile was used as the solvent; however, any solvent may be used with preference for polar solvents giving improved reaction times (Stanger K., et al. J Org Chem. 2007 72(25):9663-8; Harfenist M., et al. J Am Chem Soc 1957 79(16):4356-4358). An excess of allyl bromide was added to the solvent and continuously stirred. The sample was then submerged in the solution, and full reaction of the surface occurred within about 60 minutes, as confirmed by contact angle measurement. A reference was also measured by submerging in solvent for the duration with no reactant to ensure any changes in surface properties was due to the quaternization.

Without wishing to be bound by a particular theory, the increased hydrophobicity of the treated surfaces can be due to the presence of the allyl groups on the surface which will impart some hydrophobicity. The contact angle measurements provide information on whether or not a reaction has occurred and whether it has saturated.

The biocidal activity was tested using live bacteria cultures from a patient's mouth, which provides the full flora to act against rather than targeting an individual strain of bacteria. The bacteria was incubated on the sample surface using several bacteria film thicknesses. The thickness is defined by keeping the same interaction surface area while varying the volume of bacteria solution added. Across two separate patients and several separate growths, within 4 hours 40-50% reduction in bacteria unit counts were observed for quaternized TiN as compared to traditional Titanium implants, outperforming traditional TiN coatings. FIG. 4 shows for two separate patients a set of typical bacteria growth result of the quaternized samples. The exact efficiency varies, as each patient has different flora which varies depending on environmental factors such as hygiene, diet, and familial history.

Unless defined otherwise, all technical and scientific terms used herein have the same meanings as commonly understood by one of skill in the art to which the disclosed invention belongs. Publications cited herein and the materials for which they are cited are specifically incorporated by reference.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present disclosure without departing from the scope or spirit of the disclosure. Other aspects of the disclosure will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure disclosed herein. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the disclosure being indicated by the following claims.

Example 4

Fluralaner was added at a concentration of 100 mg/mL in IPA, with 60 kg added to 600 L of isopropanol. This composition was heated to 65° C. over 1 hour, and aged for one hour to ensure full dissolution. The solution was cooled over 20 minutes to 50° C. and seeded with 600 g of crystalline fluralaner seed, again with unmilled seed crystals having an d50 of approximately 10 μm. The batch was further cooled to 20° C. over two hours to establish the starting particles. The batch was heated to 54° C., at which point 120 L of the batch was removed and heated to an elevated temperature until fully dissolved (>65° C.). The removal rate and return rate to the crystallizer were set to approximately 4.4-4.8 L/min. The recycle loop continued for 2.75 hours, at which point the d50 particle size dimension is approximately 40 μm. The batch was aged at 54° C. for 6 hours to further relieve supersaturation, then cooled to 45° C. over 6 hours, and further cooled to 0° C. over 16 hours. See FIG. 12 for a schematic of the process equipment. The resultant slurry was filtered and dried to produce fluralaner particles. Agitation was limited during the filtration and drying. The material was delumped at low speed in a conical mill. The dried fluralaner particles were measured to determine the particle dimensions and mechanical resiliency. See FIG. 13 for the particle size distribution and mechanical resiliency. See FIG. 14 for an SEM image of the resulting particles.

Example 3

Reciprocating tests were used to characterize both friction and wear behavior of the ester blends at 25° C. and 40° C. under boundary lubrication. As mentioned prior, each ester was blended at a concentration of 1% by weight. Neat oil served as the control. The testing device is a custom ball-on-flat microtribometer as seen in FIG. 3 and was operated in conjunction with a temperature-controlled stage. In brief, precise normal loading of a probe onto the sample substrate is performed via software controlled linear stages. The sample substrate is forced to slide against the probe and subsequent lateral or frictional forces are measured. The temperature-controlled stage consists of an aluminum block that contains an oil reservoir. The block's temperature is monitored and controlled via an adhesive thermocouple connected to a PID controller. In addition, the oil temperature is monitored with a thermistor. Prior to testing, an equal volume filled the reservoir and the oil temperature was equilibrated. The oil level sits just above the substrate surface so there is a constant supply of oil into the contact zone.

Reciprocating tests were carried out using a SiC-steel interface: a 4 mm diameter silicon carbide ball on an AISI 8620 steel substrate. The ceramic was chosen for its superior hardness relative to the substrate in order to isolate the majority of the wear to the substrate and preserve the probes geometry. In this way, a consistent contact pressure can be maintained. A constant normal load of 3.4 N (maximum Hertzian pressure of 1.5 GPa) was applied as the substrate was translated at a rate of 10 mm/s over a 8 mm stroke length for 4500 cycles. The load was chosen after initial tests with the PEs at 1.0 GPa were not sufficient to generate measureable wear scars (wear depths were on the same order as the surface roughness). The substrate was isotropically polished to a finish of 0.043 μm Ra determined from a scan area of 1.41 mm×1.88 mm using a Zygo optical profilometer. Based on EHL theory, the roughness, load, and viscosity parameters placed this study well within the boundary lubrication regime as the estimated λ ratio was much less than one.

After test completion, the substrate and probes were wiped with isopropyl alcohol before undergoing SEM and EDS analysis. In addition, the substrate wear scars were scanned using the Zygo optical profilometer. Nine to eleven unique scan areas were gathered to capture the entire length of each scar. All topographic and force data was then imported into MATLAB where the average wear depth and coefficient of friction was calculated. Three replicate tests were completed for each treatment.