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The majority of Refill Friction Stir Spot Welding (RFSSW) is used to join two materials together oriented in a lap joint configuration. In this study, RFSSW was investigated and tested using an unconventional configuration setup, a hole/plug insertion approach. RFSSW was tested as a means of repairing a cracked rivet hole due to excessive use conditions. This was done by inserting a plug into a hole and using the RFSSW process to bond the plug to the base material. Machine and tool limits were investigated to determine if a refilled plug repair was possible and if complete mixing between plug/hole interface was attainable. Plug/hole homogenization was assessed via metallographic polishing of weld cross sections. Properties of the repaired aluminum alloy including both dynamic and and quasi-static tensile tests were also evaluated.

A soldagem por fricção (Friction Stir Welding - FSW) é um processo eficiente de unir ligas de alumínio de alta resistência evitando defeitos que são usualmente criados quando técnicas convencionais de soldagem são utilizadas. A indústria aeronáutica tem mostrado grande interesse neste método de soldagem, tanto para a união de ligas similares como dissimilares. Entretanto, este processo causa modificações microestruturais dependentes das condições de tratamento térmico ou termomecânico. Contato elétrico entre zonas de microestruturas diferentes, por sua vez, pode resultar em acoplamento galvânico. No presente estudo, a soldagem por FSW foi usada para unir duas ligas de alumínio dissimilares, AA2024-T3 e AA7475-T651 e o efeito desta soldagem na resistência à corrosão das juntas soldadas e na microestrutura das ligas foi avaliada. Na investigação da resistência à corrosão foram utilizados ensaios eletroquímicos, especificamente, medidas de potencial de circuito aberto (OCP) em função do tempo de exposição ao meio corrosivo, ensaios de polarização e de espectroscopia de impedância eletroquímica, global (EIS) ou local (LEIS), em duas soluções, seja 0,1 M Na2SO4 ou 0,1 M Na2SO4 + 1 mM NaCl. Os ensaios eletroquímicos evidenciaram efeito de acoplamento galvânico nas juntas soldadas. A caracterização microestrutural foi realizada por microscopia ótica, microscopia eletrônica de varredura, microscopia eletrônica de transmissão e por calorimetria diferencial. As zonas afetadas pela solda tiveram importantes modificações na microestrutura indicadas pela precipitação e dissolução de precipitados que afetam a resistência à corrosão localizada. A resistência à corrosão intergranular e a resistência à esfoliação das juntas soldadas também foram avaliadas e comparadas com as das ligas AA2024-T3 e AA7475-T651 não soldadas. Os resultados mostraram aumento da suscetibilidade das juntas soldadas a estas formas de corrosão em comparação com as ligas não soldadas sendo observado ataque mais severo na liga AA7475-T651. A identificação das áreas anódicas e catódicas resultantes do acoplamento galvânico nas juntas soldadas foi realizada por teste que consistiu na deposição de camada de gel (ágar-ágar) com indicador universal na superfície das ligas soldadas. A liga AA2024-T3 atuou como cátodo, enquanto a AA7475-T651, como ânodo no par galvânico. Além disso, evolução de hidrogênio foi observada na região de interface entre a zona termomecanicamente afetada e a termicamente afetada da liga AA7475-T651 mostrando que reações catódicas também ocorreram localmente nesta última liga. Resultados de LEIS obtidos nas diferentes zonas das duas ligas soldadas por FSW mostraram acoplamento galvânico na interface entre elas para tempos curtos de ensaio e deslocamento da região mais ativa com o tempo de ensaio para a liga AA7475-T651, mais precisamente para a interface entre a zona termomecanicamente afetada e a térmicamente afetada desta liga. / Friction Stir Welding (FSW) is an efficient process of joining high strength aluminum alloys avoiding defects that are usually created when conventional welding techniques are used. The aircraft industry has shown great interest in this welding method, both for welding of similar or dissimilar alloys. However, this process causes microstructural changes that are dependent on the thermal or thermomechanical conditions applied. Electrical contact between zones of different microstructures, in turn, can result in galvanic coupling. In the present study, FSW was used to join two dissimilar aluminum alloys, AA2024-T3 and AA7475-T651 and the effect of this process on the corrosion resistance of the welded joints and on the microstructure of the alloys was evaluated. For corrosion resistance evaluation, electrochemical tests were used, specifically, open circuit potential measurements (OCP) as a function of time of exposure time to the corrosive environment, polarization tests, and electrochemical impedance spectroscopy, global (EIS) or local (LEIS), in two solutions, either 0.1 M Na2SO4 or 0.1M Na2SO4 + 1 mM NaCl. The electrochemical tests showed galvanic coupling effects in the welded joints. Microstructural characterization was carried out by optical microscopy, scanning electron microscopy, transmission electron microscopy and differencial scanning calorimetry. The welded affected zones showed significant microstructural changes indicated by precipitation and dissolution of precipitates that affect the localized corrosion resistance. Intergranular and exfoliation corrosion resistance of the welded joints were also evaluated and compared to those of unwelded AA2024-T3 and AA7475-T651 alloys. The results showed increased susceptibility of welded joints to these forms of corrosion in comparison with the unwelded alloys with more severe attack associated to the AA7475-T651 alloy. Identification of anodic and cathodic areas due to galvanic coupling in the welded joints was evaluated by a test consisting in depositing a gel layer (ágar-ágar) with universal indicator on the surface of the welded alloys. The AA2024-T3 alloy worked as cathode, while the AA7475-T651 as anode in the galvanic coupling. Furthermore, hydrogen evolution was observed at the interface region between the thermomechanically affected zone and the heat affected alloy AA7475-T651 showing that cathodic reactions also occurred on this last alloy. LEIS results obtained in different zones of the two FSW welded alloys showed galvanic coupling at the interface between them for short test times and displacement of the most active region to the AA7475-T651 alloy, at longer periods of test, specifically to the interface between the thermomechanically affected and the heat affected zones of this last alloy.

A soldagem por fricção (Friction Stir Welding - FSW) é um processo eficiente de unir ligas de alumínio de alta resistência evitando defeitos que são usualmente criados quando técnicas convencionais de soldagem são utilizadas. A indústria aeronáutica tem mostrado grande interesse neste método de soldagem, tanto para a união de ligas similares como dissimilares. Entretanto, este processo causa modificações microestruturais dependentes das condições de tratamento térmico ou termomecânico. Contato elétrico entre zonas de microestruturas diferentes, por sua vez, pode resultar em acoplamento galvânico. No presente estudo, a soldagem por FSW foi usada para unir duas ligas de alumínio dissimilares, AA2024-T3 e AA7475-T651 e o efeito desta soldagem na resistência à corrosão das juntas soldadas e na microestrutura das ligas foi avaliada. Na investigação da resistência à corrosão foram utilizados ensaios eletroquímicos, especificamente, medidas de potencial de circuito aberto (OCP) em função do tempo de exposição ao meio corrosivo, ensaios de polarização e de espectroscopia de impedância eletroquímica, global (EIS) ou local (LEIS), em duas soluções, seja 0,1 M Na2SO4 ou 0,1 M Na2SO4 + 1 mM NaCl. Os ensaios eletroquímicos evidenciaram efeito de acoplamento galvânico nas juntas soldadas. A caracterização microestrutural foi realizada por microscopia ótica, microscopia eletrônica de varredura, microscopia eletrônica de transmissão e por calorimetria diferencial. As zonas afetadas pela solda tiveram importantes modificações na microestrutura indicadas pela precipitação e dissolução de precipitados que afetam a resistência à corrosão localizada. A resistência à corrosão intergranular e a resistência à esfoliação das juntas soldadas também foram avaliadas e comparadas com as das ligas AA2024-T3 e AA7475-T651 não soldadas. Os resultados mostraram aumento da suscetibilidade das juntas soldadas a estas formas de corrosão em comparação com as ligas não soldadas sendo observado ataque mais severo na liga AA7475-T651. A identificação das áreas anódicas e catódicas resultantes do acoplamento galvânico nas juntas soldadas foi realizada por teste que consistiu na deposição de camada de gel (ágar-ágar) com indicador universal na superfície das ligas soldadas. A liga AA2024-T3 atuou como cátodo, enquanto a AA7475-T651, como ânodo no par galvânico. Além disso, evolução de hidrogênio foi observada na região de interface entre a zona termomecanicamente afetada e a termicamente afetada da liga AA7475-T651 mostrando que reações catódicas também ocorreram localmente nesta última liga. Resultados de LEIS obtidos nas diferentes zonas das duas ligas soldadas por FSW mostraram acoplamento galvânico na interface entre elas para tempos curtos de ensaio e deslocamento da região mais ativa com o tempo de ensaio para a liga AA7475-T651, mais precisamente para a interface entre a zona termomecanicamente afetada e a térmicamente afetada desta liga. / Friction Stir Welding (FSW) is an efficient process of joining high strength aluminum alloys avoiding defects that are usually created when conventional welding techniques are used. The aircraft industry has shown great interest in this welding method, both for welding of similar or dissimilar alloys. However, this process causes microstructural changes that are dependent on the thermal or thermomechanical conditions applied. Electrical contact between zones of different microstructures, in turn, can result in galvanic coupling. In the present study, FSW was used to join two dissimilar aluminum alloys, AA2024-T3 and AA7475-T651 and the effect of this process on the corrosion resistance of the welded joints and on the microstructure of the alloys was evaluated. For corrosion resistance evaluation, electrochemical tests were used, specifically, open circuit potential measurements (OCP) as a function of time of exposure time to the corrosive environment, polarization tests, and electrochemical impedance spectroscopy, global (EIS) or local (LEIS), in two solutions, either 0.1 M Na2SO4 or 0.1M Na2SO4 + 1 mM NaCl. The electrochemical tests showed galvanic coupling effects in the welded joints. Microstructural characterization was carried out by optical microscopy, scanning electron microscopy, transmission electron microscopy and differencial scanning calorimetry. The welded affected zones showed significant microstructural changes indicated by precipitation and dissolution of precipitates that affect the localized corrosion resistance. Intergranular and exfoliation corrosion resistance of the welded joints were also evaluated and compared to those of unwelded AA2024-T3 and AA7475-T651 alloys. The results showed increased susceptibility of welded joints to these forms of corrosion in comparison with the unwelded alloys with more severe attack associated to the AA7475-T651 alloy. Identification of anodic and cathodic areas due to galvanic coupling in the welded joints was evaluated by a test consisting in depositing a gel layer (ágar-ágar) with universal indicator on the surface of the welded alloys. The AA2024-T3 alloy worked as cathode, while the AA7475-T651 as anode in the galvanic coupling. Furthermore, hydrogen evolution was observed at the interface region between the thermomechanically affected zone and the heat affected alloy AA7475-T651 showing that cathodic reactions also occurred on this last alloy. LEIS results obtained in different zones of the two FSW welded alloys showed galvanic coupling at the interface between them for short test times and displacement of the most active region to the AA7475-T651 alloy, at longer periods of test, specifically to the interface between the thermomechanically affected and the heat affected zones of this last alloy.

Composite materials are multifunctional materials having unique mechanical and physical properties that can be tailored to meet the requirements of a particular application. Aluminium based Metal Matrix Composites (MMC) always draw the attention of researchers due to its unique characteristics such as better strength to weight ratio, low wear rate and lower thermal expansion coefficient. There are various methods for manufacturing of MMC that can be grouped into two major categories: (a) Solid sate method such as powder metallurgy, co-extrusion and (b) Liquid state method such as stir casting. All of these methods for production of composites have their own advantages and disadvantages. Porosity, and poor wettabilty of dispersoids with matrix are few common problems in solid state route. Formations of undesirable phases, and segregation of dispersoids are common problems in liquid state processing route. Friction Stir Processing (FSP) technique, a derivative technique of Friction Stir Welding (FSW) has emerged as a major solid state technique to produce composites. However, there are several challenges associated with it. Most of the past work has been on limited volume of material. Researchers have tried to combine FSP technique with powder metallurgy technique to overcome aforementioned challenges associated with these techniques. Where on one hand, powder metallurgy ensures the uniform dispersion of dispersoids in the matrix, on the other hand FSP on sintered billet removes the pores and other defects. The combination of these two techniques leads to a more controlled and uniform properties. However, at the same time, it can be noted that the combination of these processes is tedious and time consuming. In this study, an attempt is made to achieve bulk dispersion of a second phase into an aluminium matrix using FSP technique. A 5 mm thickness composite is attempted in this work. To achieve this objective proper and uniform mixing of the particles is required. To achieve this, new tools and processing steps are to be designed and analyzed for a better understanding of material flow around the tool pin and the effect of different tool pin geometries on the material flow. Keeping this objective, a detailed study is carried out on material flow during FSW process using aluminium as base metal. A marker material technique is employed to understand the material flow. A strip of copper is selected as the marker material. Material flow can be qualitatively predicted during the process by observing the distribution of marker material in the weld nugget. Three different kinds of tools, each with an additional feature are designed for this purpose (a) Plain frustum shape pin (b) threaded frustum shape pin and, (c) Triflute pin . The material flow due to the plain pin tool can be considered as primary flow during the FSP. Three different kinds of flow zones are observed in the weld nugget in the case of plain tool. It is found that higher numbers of geometrical features (threads and flutes) not only enhance the material flow but also lead to the additional flow currents and more thorough and uniform mixing. A closer study of the weld nugget revealed that the copper marker particles and the matrix were diffusion bonded. Based on the reaction time available and temperature in the weld nugget a diffusion layer thickness of 4 nm is expected between copper and aluminium. However, the diffusion layer thickness was found to be 3.5 μm, which is nearly three orders of magnitude higher. This can be attributed to the enhancement of diffusion due to simultaneous application of strain and temperature. As copper is soluble in the aluminium, an insoluble marker material tin was used for study of flow in the weld nugget. However, the effect of insolubility and lower melting point had some unexpected effect on the processing loads. The normal load during steady state tool traverse in conventional butt-welding is found to be around 2.7 KN while it attains an average value of 14.7 KN when a thin strip of tin is sandwiched between these plates. However, a drop in the torque of around 13.12 NM is observed when tin was sandwiched between the plates as compared to the case when no insert was present. On closer examination of the flow behavior, it is seen that the tin melted, squeezed out and formed a lubricious layer between the tool and the work piece. This reduced the torque significantly and a concomitant drop in temperature was observed. The interaction between the tool and the colder aluminium work piece would thus result in much larger normal and transverse load Based on the expected and unexpected results of flow pattern in the weld nugget, a new FSP tool and processing steps were developed to manufacture MMC. Tungsten, which is the highest melting point metal is chosen as the dispersing phase. Further, as tungsten has high melting point, the kinetics of intermetallics formation would be low for the given FSP processing time at the processing temperature. This would lead to tungsten acting as a more ductile strengthening particle, which is expected to should give some unique characteristics to the MMC. Tungsten powder with an average diameter of 414 nm was dispersed in aluminum matrix with three different proportions after optimizing all the process parameters. It is noted that the mechanical properties are significantly influenced as the tungsten content in the matrix increases. In practice, MMC shows relatively low ductility compared to the parent metal. However in this case the composite exhibited even better ductility than the as received aluminium plates (rolled sheets). The composite showed around 129 MPa of yield strength along with 21% ductility when tungsten content is 3.8 at.%. It is also found that the reaction between aluminum and tungsten occurs during the processing and form the Al12W intermetallic phase. Though the formation of this intermetallic phase was unlikely due to the low temperature and short time available during the process, the reaction kinetics between aluminium and tungsten would have been enhanced due to the simultaneous application of strain and temperature. Given that the metal-metal, tungsten-aluminium composite produced by FSP had unique properties and also formed intermetallics, a study on incorporation of a highly insoluble material, graphite was carried out. Further graphite with its own unique properties and very low wettability with aluminium could possibly impart completely different properties to the system. Past work on graphite aluminium composites produced by other methods did not show promise. As FSP imposes high strains at relatively high flow stresses on the processed material, it was seen that the graphite got sheared to form multi-layer graphene composites with the aluminium. The graphene sheets are formed by mechanical exfoliation of graphite particles during its incorporation in the matrix. The formation of graphene was confirmed after separating the graphite from the processed zone and TEM studies of the composite. It is seen that most of the graphite got converted into multilayer graphene. This aluminium-graphene composite exhibited enhanced ductility and UTS. As received aluminium plates exhibited only 11% ductility and around 100 MPa of UTS while this composite exhibited around 26 % ductility and 147 MPa of UTS. However, there is only a slight improvement in yield strength of this composite.

Metal fatigue is a recurring problem for metallurgists and materials engineers, especially in structural applications. It has been responsible for many disastrous accidents and tragedies in history. Understanding the micro-mechanisms during cyclic deformation and combating fatigue failure has remained a grand challenge. Environmental effects, like temperature or a corrosive medium, further worsen and complicate the problem. Ultimate design against fatigue must come from a materials perspective with a fundamental understanding of the interaction of microstructural features with dislocations, under the influence of stress, temperature, and other factors. This research endeavors to contribute to the current understanding of the fatigue failure mechanisms. Cast aluminum alloys are susceptible to fatigue failure due to the presence of defects in the microstructure like casting porosities, non-metallic inclusions, non-uniform distribution of secondary phases, etc. Friction stir processing (FSP), an emerging solid state processing technique, is an effective tool to refine and homogenize the cast microstructure of an alloy. In this work, the effect of FSP on the microstructure of an A356 cast aluminum alloy, and the resulting effect on its tensile and fatigue behavior have been studied. The main focus is on crack initiation and propagation mechanisms, and how stage I and stage II cracks interact with the different microstructural features. Three unique microstructural conditions have been tested for fatigue performance at room temperature, 150 °C and 200 °C. Detailed fractography has been performed using optical microscopy, scanning electron microscopy (SEM) and electron back scattered diffraction (EBSD). These tools have also been utilized to characterize microstructural aspects like grain size, eutectic silicon particle size and distribution. Cyclic deformation at low temperatures is very sensitive to the microstructural distribution in this alloy. The findings from the room temperature fatigue tests highlight the important role played by persistent slip bands (PSBs) in fatigue crack initiation. At room temperature, cracks initiate along PSBs in the absence of other defects/stress risers, and grow transgranularly. Their propagation is retarded when they encounter grain boundaries. Another major finding is the complete transition of the mode of fatigue cracking from transgranular to intergranular, at 200 °C. This occurs when PSBs form in adjacent grains and impinge on grain boundaries, raising the stress concentration at these locations. This initiates cracks along the grain boundaries. At these temperatures, cyclic deformation is no longer microstructure- dependent. Grain boundaries don’t impede the progress of cracks, instead aid in their propagation. This work has extended the current understanding of fatigue cracking mechanisms in A356 Al alloys to elevated temperatures.

The Friction Stir Welding (FSW) process has been under constant developmentsince its invention, more than 20 years ago. Whereas most industrial applicationsuse a gantry machine to weld linear joints, there are applications which consistof complex three-dimensional joints, requiring more degrees of freedom fromthe machines. The use of industrial robots allows FSW of materials alongcomplex joint lines. There is however one major drawback when using robotsfor FSW: the robot compliance. This results in vibrations and insufficient pathaccuracy. For FSW, path accuracy is important as it can cause the welding toolto miss the joint line and thereby cause welding defects.The first part of this research is focused on understanding how welding forcesaffect the FSW robot accuracy. This was first studied by measuring pathdeviation post-welded and later by using a computer vision system and laserdistance sensor to measure deviations online. Based on that knowledge, a robotdeflection model has been developed. The model is able to estimate thedeviation of the tool from the programmed path during welding, based on thelocation and measured tool forces. This model can be used for online pathcompensation, improving path accuracy and reducing welding defects.A second challenge related to robotic FSW on complex geometries is thevariable heat dissipation in the workpiece, causing great variations in the weldingtemperature. Especially for force-controlled robots, this can lead to severewelding defects, fixture- and machine damage when the material overheats.First, a new temperature method was developed which measures thetemperature at the interface of the tool and the workpiece, based on the thermoelectriceffect. The temperature information is used as input to a closed-looptemperature controller. This modifies primarily the rotational speed of the tooland secondarily the axial force. The controller is able to maintain a stablewelding temperature and thereby improve the weld quality and allow joining ofgeometries which were impossible to weld without temperature control.Implementation of the deflection model and temperature controller are twoimportant additions to a FSW system, improving the process robustness,reducing the risk of welding defects and allowing FSW of parts with highlyvarying heat dissipation.

<p>Solid state Friction stir welding (FSW) is of major interest in the welding of aluminium since it improves the joint properties. Many applications where Al-alloys are used are subject to varying load conditions, making fatigue failure a critical issue. In the scope of this thesis, the fatigue performance of friction stir welded AlMgSi-alloy 6082 has been investigated. Static and dynamic properties of different joint configurations and welds produced with varying process parameters have been determined. Microstructures of fractured surfaces have been studied to evaluate the effect of weld discontinuities on fatigue. The mechanical strength of the friction stir welds was set in relation to that of conventional fusion welds, and that of other FS welded Al-alloys.</p><p>The friction stir process produced aluminium butt welds with high and consistent fatigue strengths, which exceeded the strengths of similar fusion welded samples. A smooth weld geometry showed to be of great importance for the fatigue performance, favouring the friction stir welds. Welding speed in a tested range of 0.35-1.4 m/min had only a modest influence on the properties of the friction stir welds; properties were not deteriorating at the highest speed. The softening of the alloy around the weldline was modelled. A fair description of the hardness profiles across the weld was obtained. At a low and high welding speed a full and partial softening respectively was predicted, indicating that full softening is not required to obtain a flawless weld.</p><p>In case of friction stir overlap welds, tool design is even more important than in butt welding to secure weld quality. A broad tool shoulder with a concave pin end gave the best performance. In particular, the minimal influence on the sheet interface when welding with such a tool was beneficial for the fatigue strength. The stress distribution in overlap and T-type test specimens has been modelled. The stress intensity factors were determined. The corresponding crack propagation rates were in fair accordance with the experimental results. It was found that a simplified approach, developed to estimate ∆K for overlap spot welds, could be used also for friction stir overlap joints.</p>

Multi-material structures are increasingly used in vehicle bodies to reduce weight of cars. The use of these lightweight structures is driven by requirements to improve fuel economy and reduce CO2 emissions. The automotive industry has replaced conventional steel components by lighter metals such as aluminium alloy. This is done together with cutting weight of structures using more advanced strength steels. However, sound joining is still difficult to achieve due to differences in chemical and thermal properties.   This research aims to develop a new innovative welding technique for joining aluminium alloy to ultra-high strength steels. The technique is based on friction stir welding process while the non-consumable tool is made of an ordinary tool steel. Welding was done by penetrating the rotating tool from the aluminium side without penetrating into the steel surface. One grade of Al-Mg aluminium alloy was welded to ultra-high strength steels under lap joint configuration. Different types of steel surface coatings including uncoated, hot-dipped galvanised and electrogalvanised coating have been studied in order to investigate the influence of zinc on the joint properties. The correlation among welding parameters, microstructures, intermetallic formation and mechanical properties are demonstrated in this thesis.  Results have shown that friction stir welding can deliver fully strong joints between aluminium alloy and ultra-high strength steels. Two intermetallic phases, Al5Fe2 and Al13Fe4, were formed at the interface of Al to Fe regardless of surface coating conditions. The presence of zinc can improve joint strength especially at low heat input welding due to an increased atomic bonding at Al-Fe interface. The formation of intermetallic phases as well as their characteristics has been demonstrated in this thesis. The proposed welding mechanisms are given based on metallography investigations and related literature. / <p>QC 20170519</p>

Identifying the best control method for problematic wildlife is an ever present issue in wildlife management. Popular control methods have ranged from lethal techniques, extirpating the animal, to multiple non-lethal methods focused on deterring undesired behavior. In the past, lethal methods were the preferred choice. However, with increased awareness of the need for biodiversity conservation, new management methods focus on non-lethal control, with emphasis on exploiting aspects of naturally occurring organismal behaviors and ecology. Over the past decade, technological advances in extraction method’s and equipment have also developed new techniques providing a broader range of information about species biology for management use. One of the most well documented conflicts between wildlife and humans is that of the wolf. Using advanced technology and new techniques, we investigated the implication of using chemosensory signals in canid urine to modify behavior as a possible non-lethal alternative in large predator management. Here we used the SBSE method coupled with improved GC/MS equipment to analyze the volatile organic compounds in the urine of four canid species, gray wolf (Canis lupus), red wolf (Canis rufus), wolf-dog hybrids (Canis familiaris) and the domestic dog (Canis familiaris) in order to create working urinary profiles. The extraction method identified several compounds also seen in the urinary profiles of other large predators. In addition, similarities and differences were also noted between taxa and the sexes, and these can be further explored in future studies. Two identified urinary compounds, acetophenone and methyl propyl sulfide, were selected for further behavioral evaluation. We focused on these compounds and their influence as chemosensory signals triggering urine marking events in both the gray wolf and red wolf. Behavioral observations of the effects of these two chemicals indicated they elicited responses from captive wolves. At each of the three study sites, the combination of these chemicals produced urine-marking events along the territory boundary by dominant animals. As a result, the investigation focused on what triggered the urine-marking events, the chemicals themselves, their combination, or the breakdown of the chemicals producing other odorants. It was found that there was no significant degradation of the chemicals over time and environmental conditions produced no significant breakdown of the acetophenone prior to the addition of methyl propyl sulfide. This posed a number of new questions and illustrated the need for additional behavioral studies. The results of this study analyzing chemosensory signals in canid urine, provides biologists with new information to aid in the development of new non-lethal management strategies for handling problematic wildlife as well as providing useful information for future research involving reproduction, predator/prey dynamics, territory maintenance, and a host of other studies focusing on animal ecology in association with chemosensory signaling.