COMPOSITE PARTICLE, METHOD OF FORMATION OF AN ARTICLE AND ARTICLE

专利摘要:
method of controlling the corrosion rate of alloy particles, alloy particle with controlled corrosion rate and articles comprising the particle. the present invention relates to a composite particle comprising a core, a protective layer deposited on the core, and additionally comprising a region between layers formed at an interface of the protection layer and the core, the region between layers having a reactivity smaller than that of the core, and the protective layer having a lower reactivity than that of the region between layers, the metallic layer not identical to the protective layer and deposited in the protective layer, the metallic layer having a lower reactivity than that of the core, and optionally, a layer of adhesion metal deposited on the metal layer.
公开号:BR112014001466B1
申请号:R112014001466-3
申请日:2012-07-18
公开日:2021-04-27
发明作者:Oleg A. Mazyar；Michael Johnson；Randall Guest；Nicholas Carrejo；Wayne Furlan；Sean Gaudette；Zhiyue Xu
申请人:Baker Hughes Incorporated；
IPC主号:

专利说明:

Cross Reference to Related Orders
[0001] The present application claims the benefits of U.S. application No. 13/194271, filed on July 29, 2011, which is incorporated herein by reference in its entirety. Background
[0002] Certain downhole operations involve placing elements in a downhole environment, where the element performs its function, and is then removed. For example, elements such as ball assemblies / ball settings and fracturing plugs (frac) are downhole elements used to seal lower areas in a well bore in order to carry out a hydraulic fracturing process (also referred to in the art) as "fracturing") to fracture different zones of reservoir rock. After the fracturing operation, the ball / ball seat or plugs are then removed to allow fluid to flow to or from the fractured rock.
[0003] Spheres and / or spherical seating, and frac buffers, can be formed from a corrosive material so that they do not need to be physically removed intact from the downhole environment. Thus, when the operation involving the ball / ball seat or frac buffer is completed, the ball, ball seat, and / or frac buffer will corrode. Otherwise, the downhole article may have to remain in the well for a longer period than is necessary for the operation.
[0004] To facilitate removal, said elements can be formed of a material that reacts with the well-bottom environment, so that they do not need to be physically removed, for example, by a mechanical operation, but can instead addition, if it corrodes or dissolves under rock bottom conditions. However, although the corrosion coefficients, for example, of an alloy used to prepare a corrosive article can be controlled by adjusting the composition of the alloy, an alternative way of controlling the corrosion rate of a downhole article is desirable.
[0005] Corrosible materials may include those having a high activity in the galvanic salt water series, such as a magnesium alloy adjusted for the corrosion rate. It was observed that adjusting the amount of trace contaminants in the magnesium alloy can have a significant impact on the corrosion rate of these alloys (Song, G. and Atrens, A., "Understanding Magnesium Corrosion: A Framework for Improved Alloy Performance," Adv. Eng. Mater. 2003, 5 (12) pp. 837 - 858). For example, metals such as nickel, iron, copper, calcium, etc., can be added to magnesium to increase the corrosion rate and other metals such as zirconium, yttrium, etc. can be added to reduce the corrosion coefficient. By balancing the amounts of said additives to achieve a desired volume of corrosion rate, you can thereby control the general corrosion of articles produced from the alloy; however, this approach requires the preparation of multiple alloy batches, requiring a high batch-to-batch reproduction capacity and precise reproducibility control of metal additives or contaminants in the alloy.
[0006] Thus, there is still a need to control the overall corrosion rate of magnesium alloys for use in downhole articles without the need for fine adjustment of the alloy composition and with improved corrosion control. summary
[0007] The above deficiencies and other deficiencies of the prior art are overcome by, in one embodiment, a composite particle comprising a core, a protective layer deposited on the core, and additionally comprising a region between layers formed at an interface of the layer of protection and the core, the region between layers having a lower reactivity than that of the core, and the protection layer having less reactivity than that of the region between layers, a metallic layer not identical to the protective layer and deposited in the layer of protection, the metallic layer having a lower reactivity than that of the core, and optionally, an adhesion metal layer deposited on the metallic layer.
[0008] In another embodiment, the composite particle comprises a magnesium-aluminum alloy core, the protective layer comprising a layer deposited on the aluminum-containing core, and additionally comprising a region between layers comprising α-Mg and Y — Mgi7Ali2 formed at the interface between the magnesium alloy core and the aluminum-containing layer, and further comprising inclusions of alumina, magnesium, or a combination comprising at least one of said oxides, the metallic layer deposited on the protective layer, the metallic layer comprising Ni, Fe, Cu, Co, W, alloys thereof, or a combination comprising at least one of the aforementioned, a protective layer containing aluminum deposited on the metallic layer, and optionally, a layer containing adhesion metal aluminum, in which the region between layers, protective layer, metallic layer, and optional adhesion metal layer are inter-dispersed with respect to each other.
[0009] In another embodiment, a method of adjusting the corrosion rate in an aqueous electrolyte is described for a composite particle having a core, a protective layer deposited on the core, and additionally comprising a region between layers formed at an interface of the protective layer and the core, the region between layers having less reactivity than that of the core, and the protection layer having less reactivity than that of the region between layers, the metallic layer not identical to the protection layer and deposited in the protective layer, the metallic layer having a lower reactivity than that of the core, and optionally, an adhesion metal layer deposited on the metallic layer, the method comprising selecting the metallic layer so that the lower the reactivity of the metallic layer is with respect to the protective layer, the higher the corrosion rate, and select the quantity, thickness, or both quantities and thicknesses of the protective layer and metallic layer so that the smaller the quantity, thickness, or both the quantity and thickness of the protective layer in relation to those of the metallic layer, the higher the corrosion rate. Brief Description of Drawings
[0010] With reference now to the drawings in which similar elements are numbered similarly in the various Figures:
[0011] Figure 1 shows a cross-sectional view of a composite particle 100a having a multilayer structure (Figure 1A) and a cross-sectional view of a composite particle 100b having an interdispersed layer (Figure 1B);
[0012] Figure 2 shows a cross-sectional view of a composite particle 200a having a multilayer structure (Figure 2A) and a cross-sectional view of a composite particle 200b having an interdispersed layer (Figure 2B); and
[0013] Figure 3 shows a cross-sectional view of an example of a corrosive downhole article 300 prepared from composite particles 310. Detailed Description of the Invention
[0014] Described here is a composite particle useful for making a corrosive article. The composite particle has a multilayer structure of a core of a highly reactive material, such as magnesium or magnesium alloy, coated with a protective layer such as, for example, aluminum. At the interface of the protective layer and the core, an intermetallic phase can form, such as a crystalline metallic compound of magnesium and aluminum, and present in discontinuous regions. The protective layer, which includes the intermetallic regions, has a layer of a noble material with a lower reactivity (that is, more noble than the protective layer, although comparable in reactivity to the intermetallic phase) disposed therein. An additional layer of an adhesive metal, for example, aluminum, can be placed on top of the noble material layer, to provide adhesion between particles with the molding. The region between layers, protective layer, noble material layer (referred to here as the "metallic layer", where the noble material is a metal), and optional adhesion layer are believed to be interdispersed with each other, and form an outer shell of varying composition that is also inter-dispersed with the core.
[0015] The noble material layer, which has a lower reactivity with respect to the core material, acts as a cathode, while the core, produced from a metal such as magnesium which is more reactive than the noble metal layer , is anodic with respect to the noble metal layer. The protective layer, which includes the intermetallic phase, is also cathodic with respect to the core, but anodic with respect to the noble metal layer. A galvanic discharge cycle (eg, corrosion) occurs between relatively anodic and relatively cathodic materials in the presence of an electrolyte. By adjusting the composition of the noble metal layer with respect to the core and the protective layers, and by adjusting the quantities and / or thicknesses of the protective and noble metal layers, the corrosion rate of the composite particle is adjusted.
[0016] Composite particles are formed into articles by compressing and forming the particles using, for example, cold molding followed by forging.
[0017] The core includes any material suitable for use in a downhole environment, as long as the core is corrosible in the downhole environment with respect to the second material having a different reactivity. In one embodiment, the composite particle thus includes a magnesium-containing core. A magnesium-containing core includes any alloy that is corrosive in a corrosive environment, including those typically found at the bottom of the well, such as an aqueous environment that includes salt (ie, brine), or an acidic or corrosive agent such as hydrogen sulfide , hydrochloric acid, or other corrosive agents. Suitable magnesium alloys for use include magnesium (Mg) alloys with aluminum (Al), cadmium (Cd), calcium (Ca), cobalt (Co), copper (Cu), iron (Fe), manganese (Mn), nickel (Ni), silicon (Si), silver (Ag), strontium (Sr), thorium (Th), zinc (Zn), zirconium (Zr), or a combination comprising at least one of the said elements. Particularly useful alloys include magnesium alloy particles including those prepared from magnesium with an alloy of Ni, W, Co, Cu, Fe, or other metals. Alloy or trace elements can be included in varying amounts to adjust the corrosion rate of magnesium. For example, four of the aforementioned elements (cadmium, calcium, silver, and zinc) have mild to moderate acceleration effects on corrosion coefficients, while four others (copper, cobalt, iron, and nickel) have an acceleration effect on corrosion. Examples of commercially available magnesium alloys that include different combinations of the above alloying elements to achieve different degrees of corrosion resistance include, but are not limited to, for example, magnesium with aluminum alloy, strontium, and manganese such as alloys. AJ62, AJ50x, AJ51x, and AJ52x, and magnesium with aluminum alloy, zinc, and manganese including AZ91A-E alloys.
[0018] It will be seen that alloys having higher corrosion coefficients than those of the exemplary alloys above are contemplated as being useful here. For example, nickel has been found to be useful in reducing the corrosion resistance (that is, it increases the corrosion rate) of magnesium alloys when included in amounts less than or equal to about 0.5% by weight, specifically less than that or equal to about 0.4% by weight, and more specifically less than or equal to about 0.3% by weight, to provide a useful corrosion rate for the downhole corrodible article. In another embodiment, the magnesium-containing core comprises a magnesium-aluminum alloy.
[0019] Particle sizes for magnesium alloy cores can be from about 50 to about 150 micrometers (μm), more specifically about 60 to about 140 μm, and even more specifically about 70 to about 130 μm. Useful magnesium alloys may include combinations of the above elements and / or contaminants sufficient to achieve a corrosion rate for the magnesium alloy core of about 0.1 to about 20 mg / cm2 / hour, specifically about 1 to about 15 mg / cm2 / hour using a 3% by weight aqueous solution of KCl at 93 ° C (200 ° F).
[0020] The composite particle includes a protective layer. The protective layer is formed when depositing on the core, a material having a lower reactivity than that of the core. In an example of a modality, the protective layer is a layer deposited on the aluminum-containing core. In one embodiment, the core is a magnesium alloy core and the protective layer is a layer containing aluminum. As used here "in" and "deposited in" means that the layer may or may not be in direct contact with, the underlying surface to which the layer is applied, unless otherwise specified when determining that the layers are at least partially in contact. It will be further understood that "deposited" and "depositing," when used in relation to a method, indicates the deposition action, while "deposited" when used in the context of a composition or article, merely indicates the juxtaposition of the layer with respect to to the substrate and does not indicate a deposition process. The protective layer additionally comprises a region between layers formed at the interface of the core and the protective layer, which is derived in terms of composition from the core and the protective layers. In one embodiment, the region between the layers formed at the boundaries of a magnesium-containing core and a protective layer containing aluminum, and the region between the layers comprises an intermetallic compound. For example, magnesium-aluminum alloys include an α-Mg phase, and in addition, an intermetallic Y-Mgi7Ali2 phase that accumulates at the grain boundaries within the Mg-Al alloy. The Y-Mgi7Ali2 intermetallic phase is generally present in amounts less than 30% by weight of the Mg-Al alloy. Depending on the composition, additional phases may also be present, including solid Al solution, and other intermetallic phases such as β-Mg2Al3. With the deposition of the protective layer containing aluminum, the Y — Mgi7Ali2 phase forms and also accumulates at the interface of the protective layer and in the nucleus containing Mg. Heat treatment can accelerate the formation of the region between layers. For example, heating to temperatures lower than the eutectic point (for example, less than or equal to about 450 ° C, depending on the composition of the alloy, and as long as the eutectic point is not exceeded) for about 15 minutes it can form an intermetallic phase at the interface of the nucleus containing Mg and the layer containing Al. The composite particle thus includes, as part of the region between layers, the intermetallic compound Y-Mgi7Ali2. The region between layers forms throughout the contact area of the nucleus containing Mg and the layer containing Al, or a portion of the contact areas. The deposition method and any heat treatment can be adjusted so that the intermetallic phase intervenes between a portion of contact surfaces of the alloy core containing Mg and the layer containing Al. The protective layer additionally includes an oxide of one or more of the metals of which the core and / or protective layers are comprised. For example, where the core comprises magnesium or a magnesium-aluminum alloy, and the protective layer comprises aluminum, the protective layer optionally includes magnesium oxides (such as magnesium), aluminum (such as alumina), or a combination comprising at least one of the above.
[0021] The composite particle additionally includes a metallic layer not identical to the protective layer and deposited in the protective layer. The metallic layer has a lower reactivity with respect to the core, based on the series of galvanic salt water from the lower reactivity (that is, more noble metals) to high reactivity (that is, less noble metals). In one embodiment, the metal (s) used for the metallic layer allows hydrogen to form when used as a cathode in an electrochemical cell. The metallic layer thus comprises a transition metal of group 6-11. Specifically, the transition metal of group 6-11 includes Ni, Fe, Cu, Co, W, alloys thereof, or a combination comprising at least one of the above.
[0022] The composite particle optionally includes an adhesion layer deposited on the metallic layer. The adhesion layer comprises a material that promotes adhesion between the composite particles. An example of the adhesion layer includes aluminum or an aluminum alloy. When compressing and forging the composite particles coated with adhesion layer to form a molded article, the particles bond to each other through contact between particles via the material of the adhesion layer, to additionally provide mechanical resistance to the article.
[0023] The layers (protective layer, metallic layer, and optional adhesion layer) can each have an average thickness of about 0.05 to about 0.15 μm, and specifically about 0.07 to about 0.13 μm. In one embodiment, each layer does not completely cover the underlying layer, and the layer coverage is thus discontinuous. Additionally, where the layers are "in one another", interstitial spaces at the layers' interfaces may be present. In one embodiment, the region between the layers, the protective layer, the metallic layer, and the optional bonding metal layer are interdispersed with each other. As used here, "interdispersed" means that two or more adjacent layers interpenetrate or are through each other in an intimate mixture, where it will be observed that two (or more) interdispersed layers have, on average, a gradient of composition due to the interpenetration of a layer in the adjacent layer.
[0024] The core and the protective layer, the protective layer and the metallic layer, and the metallic layer and optional adhesion layer, are each so in partial mutual contact, and are interdispersed, so that the components the core, the protective layer, and the metallic layer are present on the exposed surface of the composite particle.
[0025] In one embodiment, the composite particles have a corrosion rate of about 0.1 to about 20 mg / cm2 / hour, specifically about 1 to about 15 mg / cm2 / hour using an aqueous solution of 3% by weight KCl at 200 ° F (93 ° C).
[0026] In a specific embodiment, the protective layer is a layer containing aluminum, and the core is a core containing magnesium. In one embodiment, the protective layer comprises aluminum. In another embodiment, the protective layer additionally comprises, in addition to aluminum, inclusions of alumina, magnesium, or a combination comprising at least one of said oxides. The protective layer additionally includes a region between the layers formed at the interface between the magnesium alloy core and the first aluminum-containing layer. In one embodiment, the region between layers comprises Y-Mgi7Ali2.
[0027] Also in a specific modality, the metallic layer comprises a transition metal of group 6-11 in the protective layer. The transition metal of group 6-11 includes Ni, Fe, Cu, Co, W, alloys thereof, or a combination comprising at least one of the above.
[0028] Optionally, in a specific modality, the adhesion layer is a layer containing aluminum deposited on the metallic layer.
[0029] Deposition of the protective, metallic, and adhesion layers on the core is not particularly limited. Where either or both of the optional protection and adhesion layer include aluminum or an aluminum alloy, uniformly depositing on the aluminum layer (s) in the magnesium alloy core particle is carried out in an exemplary decomposition modality. an organometallic compound, such as triethyl aluminum (having a boiling point of 128-130 ° C at 50 mm Hg), after introducing the organometallic compound into a fluidized bed reactor containing the magnesium alloy core particle to deposit the layer of protection, or the introduction of the organometallic compound in a reactor containing particles of magnesium alloy core / protective layer / metallic layer to deposit the adhesion layer. The interlayer region, which in this case includes an intermetallic compound such as Y-Mgi7Ali2, additionally forms at the interface of the alloy core containing Mg and the protective layer by heat treatment, such as sintering and / or annealing, and / or the forging of an article molded from the composite particles, at a temperature below the melting point of all or part of the composite particle.
Similarly, the deposition of the uniform metallic layer is also not particularly limited, and can be carried out, for example, by decomposing an organometallic compound (such as carbonyl nickel where the metallic layer is nickel) after introducing the organometallic compound in a fluidized bed reactor, containing a particle of magnesium alloy core coated with the protective layer.
[0031] The core can also be coated with materials for the protective layer, the metallic layer, and the optional adhesion layer using a physical mixing method. For example, the core can be mixed with one or more components of the protective layer, the metallic layer, and the optional adhesion layer by cryo-grinding, ball-grinding, or the like. In this way, the components of the protective layer, the metallic layer and the adhesion layer can be included in sequence, or the components for the two or all three layers can be included simultaneously. Combinations of deposition methods including vapor phase deposition and physical methods can also be used to provide the composite particles. Where all components are included by physical mixing simultaneously, it will be observed that a single layer is formed which is a composite of the components of the protective layer, the metallic layer, and the adhesion layer.
[0032] In another embodiment, the core comprises an inner core of a first core material and an outer core of a second core material, the inner core material having a lower reactivity than that of the outer core. The inner core is made of any material useful for depositing a highly reactive material such as magnesium, without limitation. The inner core can thus be any suitable, low reactivity material, such as a transition metal 6-11 including Ni, Fe, Cu, Co, W, alloys thereof, or a combination comprising at least one of the above; a metal oxide such as alumina, silica, silicates, iron oxides, titania, tungstates, and the like; a polymer including a phenolic polymer; ceramics; glasses; or other such materials. In an example of an embodiment, the inner core comprises an aluminum, nickel, iron, alumina, titania or silica alloy, and the outer core comprises magnesium or a magnesium alloy as described hereinabove. The outer core is deposited on the inner core using any suitable deposition method such as physical vapor deposition (PVD) of metallic magnesium or magnesium alloy in a fluidized bed reactor. The core structure, having inner and outer cores, is then coated with the protective layer, the metallic layer, and the optional adhesion layer as described above to form the composite particle.
[0033] The composite particle in general has a particle size of about 50 to about 150 micrometers (μm), and more specifically about 60 to about 140 μm.
[0034] In another embodiment, a method of adjusting the corrosion rate of a composite particle, or article prepared from it, is described. In one embodiment, the adjustment is carried out by one or both selecting the composition of the metallic layer to present the desired reactivity, where the lower the reactivity of the metallic layer in relation to the protective layer (and by definition to both, both the region of core and interlayer), the faster the corrosion rate; and conversely, the higher the reactivity of the metallic layer with respect to the protective layer, the slower the corrosion rate. Alternatively or in addition, in one embodiment, the adjustment is performed by increasing the amount and / or thickness of the protective layer to any determined amount and / or thickness of the metallic layer. It will be further observed that the additional control of the corrosion rate is carried out by the degree of interdispersion of the core, of the interlayer region, of the protection layer, and of the metallic layer, where the more highly dispersed these layers are, the higher the rate of corrosion, and conversely, the less the layers are dispersed, the slower the corrosion rate. Thus, the amount and thickness as used here are related to the fact that the higher the amount of the layer, expressed as a percentage by weight based on the weight of the composite particle, the greater the thickness.
[0035] The surface of the composite particles includes not only anodic, but also cathodic regions of the interdispersed layers. It will be understood that "anodic regions" and "cathodic regions" are relative terms, based on the relative reactivity of the interdispersed materials. For example, as discussed above, magnesium (from the core) is anodic with respect to the cathodic intermetallic compound of the region between layers (Y-Mgi7Ali2) and cathodic aluminum from the region between layers / protective layer, and anodic with respect to nickel from the cathodic metallic layer. Similarly, the intermetallic compound (Y-Mgi7Ali2) is anodic with respect to cathodic aluminum from the protective layer, and anodic with respect to nickel from the cathodic metal layer; and aluminum from the protective layer is anodic with respect to nickel from the metallic layer. Thus, with the exposure of the composite particle surface (and any article produced from the composite particles) to an electrolyte, multiple localized corrosion mechanisms occur in which the reversal of the anodic and cathodic regions occurs. For example, after exposure, the anodic core material (such as magnesium) is corroded, a previously cathodic material (such as intermetallic compound or aluminum in the protective layer) becomes anodic and is corroded by interaction with the most metallic layer. cathodic (for example, which includes nickel, etc.). As the surface corrodes and a new, more anodic core material such as magnesium is exposed, the situation is again reversed and the aluminum or intermetallic compound becomes cathodic in relation to the core material.
[0036] As the corrosion progresses in regions located on the surface between the anodic and cathodic regions in the presence of a fluid electrolyte (water, brine, etc.), the referred regions, referred to here as microcells, can corrode outwards on the surface of the composite particle and bond to other microcells to form larger corrosion regions, which in turn can bond to other corrosion regions, etc., as additional anodic materials such as magnesium (from of the core) or intermetallic Y-Mgi7Ali2 (from the region between layers / protective layer) is exposed. After these regions are corroded, new, underlying anodic materials from the core are exposed to the electrolyte. With corrosion, said interdispersed layers can thus become permeable to the fluid electrolyte. This allows percolation of electrolytic fluids within the corrosion surface to penetrate and mine the layers, and the process is repeated until the corrosive materials are consumed. It will be noted that the presence of metal oxides at the core / protective layer interface also reduces the corrosion rate of the core at the interface by acting as an inert barrier, and thus affects the relative anodic / cathodic characteristic of the microcell (for example, where alumina and / or magnesium are present between the magnesium core and the intermetallic compound, the intermetallic compound is isolated from the core and will be anodic with respect to the metallic layer). Thus, the presence of metal oxide inclusions affects the overall corrosion rate of the composite particle.
[0037] Where the core comprises an inner and outer core in which the outer core is anodic, corrosion advances until only the inner core remains. The inner core thus exposed no longer has the structural integrity and cohesive ability of the composite particle, and is dispersed in the surrounding fluid as the particle suspension, and can be removed in this way.
[0038] Thus, in one embodiment, a method of adjusting the corrosion rate on a composite particle includes selecting the metallic layer so that the lower the reactivity of the metallic layer is with respect to the protective layer, the higher the rate of corrosion. In another embodiment, a method of adjusting the corrosion rate on a composite particle includes selecting the amount, the thickness, or both the amounts and thicknesses of the protective layer and the metallic layer so that the smaller the amount, the thickness, or both the quantity and thickness of the protective layer are in relation to those of the metallic layer, the higher the corrosion rate. The region between layers, protective layer, metallic layer, and optional adhesion metal layer being interdispersed with each other, and have compositions as discussed above.
[0039] In another embodiment, an article comprises composite particles that can be provided as a powder or other suitable form, such as a pre-compressed granule. Articles can be prepared from the composite particle by compressing or otherwise forming the composite particles, to form an article having the appropriate shape. For example, composite particles are shaped or compressed into the desired shape by cold compression using an isostatic press at about 40 to about 80 ksi (about 275 to about 550 MPa), followed by forging or sintering and machining, to provide an article having the desired shape and dimensions. As described here, forging or sintering is carried out at a temperature below that of the melting point of the components.
[0040] Thus, a method of forming an article comprises molding the composite particles and forging the shaped article.
[0041] The article thus prepared is referred to as an article of electrolytically controlled material (EMF), and useful under rock bottom conditions. Items include, for example, a ball, a ball seat, a fracturing plug, or another rock bottom item. However, it should be understood that although the aforementioned articles are described, there are other uses for composite particles in the form of powder. For example, composite particles can be included in a matrix that is not metallic, and can be applied to the surface as a coating, such as paint, powder coating, etc., where an electrolytically controlled process takes place in the presence of water. , and preferably, water plus an electrolyte. Said processes can include coatings for marine applications such as drilling rigs, boat or ship hulls, underwater tools, or other applications. Said electrolytic material can provide a sacrificial layer to mitigate or prevent corrosion of an underlying metal layer, or alternatively it can prevent the adhesion, for example, of marine organisms to the underwater surface coated with the composite particles.
[0042] An example of use is described here. Figure 1 shows in schematic cross-section different structural variants of the composite particles 100a and 100b. In Figure 1A, the composite particle 100a includes a core 110; a protective layer 120 which includes an intermetallic region 121 (heavy dotted line) and aluminum layer 122 surrounding the intermetallic region; the metal layer 130, and optionally, a second aluminum layer 140 that functions as an adhesion layer. Said adhesion layer 140 can be included to promote adhesion of the particles when compressed together to form a formed article. It will be seen that the layers, although showing a distinct core-shell layer, may also be intermixed at the interfaces and / or the layers may be discontinuous on the surfaces to which they are applied, so that the core 110 is in fact in contact with protective layer 120 and / or metallic layer 130 and / or adhesion layer 140.
[0043] In Figure 1B, the composite particle 100b has a core 110 and an interdispersed layer 150 that includes the components of the region between layers, the protective layer, the metallic layer, and the optional adhesion layer (not shown individually in the Figure 1B). It will be seen that said interdispersed structure can derive from a discontinuous core-shell structure as described in Figure 1A, and in which the interdispersion is increased by heat treatment (for example, sintering); or the interdispersed structure can be derived from a physical method of forming the particles (for example, cryo- or sphere-grinding) or by including precursor materials for more than one layer in a fluidized bed reactor during layer formation. The inter-dispersed layer 150 is homogeneously inter-dispersed with the components of the different layers (interlayer region, protective layer, metallic layer) equally distributed through the inter-dispersed layer 150, or is non-uniformly distributed, for example, in a gradient where the composition changes to starting from the composition of the interlayer region predominantly at the interface of the interdispersed layer 150 and core 110, to the composition of the adhesion layer predominantly on the external surface of the interdispersed layer 150.
[0044] Figure 2 shows, similar to Figure 1, cross-sectional views of different structural variants of the composite particles 200a and 200b. In Figure 2A, the composite particle 200a includes a core 210 comprising inner core 211 and outer core 212; the protective layer 220 which includes an intermetallic region 221 (heavy dotted line) and the aluminum layer 222 surrounding the intermetallic region; the metallic layer 230, and optionally, a second aluminum layer 240 that functions as an adhesion layer. As in Figure 1A, it will be observed that the layers, although shown as distinct layers of core-shell, can also be intermixed at the interfaces and / or the layers can be discontinuous on the surfaces to which they are applied.
[0045] In Figure 2B, the composite particle 200b has a core 210 comprising the inner core 211 and the outer core 212 and an interdispersed layer 250 that includes components of the region between layers, protective layer, metallic layer, and layer of optional adhesion (not shown individually in Figure 2B). As in Figure 1B, it will be seen that said interdispersed structure can be derived from a discontinuous core-shell structure, from crushing to form the particles, or by including precursor materials for more than one layer in a bed reactor. fluidized during layer formation. Also as in Figure 1B, the interdispersed layer composition 250 is homogeneously distributed, or is non-uniformly distributed, such as, for example, in a gradient.
[0046] In Figure 3, as an example of an article, sphere 300 is shown. In Figure 3, sphere 300 is composed of composite particles 310. During cold compaction to form sphere 300, powder particles of composite 310 are compressed inward and formed to form spherical sphere 300 with interstitial spaces 320, where the interstitial spaces 320 are further reduced in volume by forging and / or sintering to reduce the free volume from about 20% after compacting to less than about 5%, specifically less than about 3%, and still more specifically less than about 1% after forging / sintering. When used in conjunction with a ball seat (not shown) and seated in a ball seat to prevent fluid flow ahead of the ball / ball seat, the ball 300 forms a well-bottom seal to isolate, for example, a fracturing zone located below the ball / ball seating assembly.
[0047] Although one or more modalities have been shown and described, modifications and substitutions can be produced to them without deviating from the spirit and scope of the present invention. Therefore, it should be understood that the present invention has been described by way of illustration and not by limitation.
[0048] All ranges described here are inclusive of end points, and end points are independently combinable with one another. The suffix "(s)" as used here is intended to include not only the singular, but also the plural of the term it modifies, thereby including at least one of that term (for example, the dye (s) includes at least one dye) . "Optional" or "optionally" means that the event or circumstance subsequently described may or may not occur, and that the description includes cases where the event occurs and cases where it does not. As used here, "combination" is inclusive of mixtures, combinations, alloys, reaction products, and the like. All references are hereby incorporated by reference.
[0049] The use of the terms "o", "a" and "um", "an" and similar referents in the context of describing the present invention (especially in the context of the appended claims) must be constructed to cover not only the singular but also the plural, unless otherwise indicated here or clearly contradicted by the context. In addition, it should be noted that the terms "first," "second," and the like here do not denote any order, quantity, or importance, but are instead used to distinguish one element from another. The "about" modifier used in connection with the quantity is inclusive of the given value and has the meaning dictated by the context (for example, it includes the degree of error associated with the measurement of the particular quantity).

权利要求:
Claims (17)
[0001]
1. Composite particle, characterized by the fact that it comprises: a core (110), a protective layer (120) deposited on the core (110), and additionally comprising a region between layers (121) formed at an interface of the layer of protection (120) and the core (110), the region between layers (121) having a lower reactivity than that of the core (110), and the protection layer (120) having a lower reactivity than that of the region between layers (121), a metallic layer (130) not identical to the protective layer (120) and deposited in the protective layer (120), the metallic layer (130) having a lower reactivity than that of the core (110), and optionally , a layer of adhesion metal (140) is deposited on the metal layer (130); wherein at least one of the protective layer (120), the region between layers (121), the metallic layer (130) and the optional bonding metal layer (140) are discontinuous, and where the composite particle is corrosive in the presence of an electrolyte fluid.
[0002]
2. Composite particle according to claim 1, characterized in that the core (110) comprises magnesium, the protective layer (120) comprises aluminum and, optionally, aluminum oxides, magnesium, or a combination comprising at least at least one of the above, and the region between layers comprises an intermetallic compound.
[0003]
3. Composite particle according to claim 2, characterized by the fact that the intermetallic compound is Y-Mgi7Ali2.
[0004]
4. Composite particle according to claim 1, characterized by the fact that the metallic layer comprises a transition metal of group 6-11.
[0005]
5. Composite particle according to claim 4, characterized by the fact that the transition metal of group 6-11 comprises Ni, Fe, Cu, Co, W, alloys thereof, or a combination comprising at least one of the above mentioned.
[0006]
6. Composite particle according to claim 1, characterized in that the core (110) comprises an inner core (110) of a first core material and an outer core of a second core material, the core material. inner core having a lower activity than that of the outer core.
[0007]
7. Composite particle according to claim 1, characterized by the fact that the inner core comprises aluminum, and the outer core comprises magnesium.
[0008]
8. Composite particle according to claim 1, characterized in that the core (110) comprises a magnesium-aluminum alloy.
[0009]
9. Composite particle according to claim 1, characterized by the fact that the core (110) and the protective layer, the protective layer (120) and the metallic layer, and the metallic layer and the metal layer optional membership, each of which is in partial mutual contact.
[0010]
10. Composite particle according to claim 1, characterized by the fact that the region between layers, the protective layer (120), the metallic layer and the optional adhesion metal layer are inter-dispersed with each other.
[0011]
11. Composite particle according to claim 1, characterized by the fact that the protective layer (120) is cathodic with respect to the core (110), and anodic with respect to the metallic layer.
[0012]
12. Composite particle according to claim 1, characterized by the fact that the core (110) is in partial mutual contact with the protective layer (120), the metallic layer, the optional adhesion metal layer or a combination comprising at least one of the above.
[0013]
13. Composite particle according to claim 1, characterized by the fact that each of the core (110), the protective layer (120), the region between layers, the metallic layer and the optional adhesion metal layer it is discontinuous.
[0014]
14. Composite particle according to claim 1, characterized by the fact that the electrolyte comprises water or brine.
[0015]
15. Composite particle, characterized by the fact that it comprises: a magnesium-aluminum alloy core (110), and interdispersed layer (150) comprising a protective layer (120) comprising a layer containing aluminum deposited on the core (110) , the protective layer (120) further comprising inclusions of alumina, magnesium or a combination comprising at least one of these oxides; a region between layers (121) comprising Y-Mg17Al12 formed at the interface between the magnesium alloy core (110) and the aluminum-containing layer (120), and a metallic layer (130) deposited on the protective layer (120), the metallic layer (130) comprising Ni, Fe, Cu, Co, W, alloys thereof, or a combination comprising at least one of the above, and wherein: the components of the region between layers (121), protective layer (120 ) and metallic layer (130) are interdispersed with each other within the interdispersed layer (150), a protective layer (120) containing aluminum deposited on the metallic layer (130), and optionally, the interdispersed layer (150) comprises each one adhesion metal containing aluminum (140) and the components of the adhesion metal layer are also interdispersed with the components of the region between layers (121), protective layer (120) and metallic layer (130) within the interdispersed layer (150) .
[0016]
16. Method of forming an article, characterized in that it comprises molding the composite particles as defined in claim 1, and forging the molded article.
[0017]
17. Article characterized by the fact that it comprises the composite particles as defined in claim 1, wherein the article comprises a sphere, a sphere settlement or a fracturing plug

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同族专利:

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公开号 | 公开日

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AU2012290564A1|2014-01-16|

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CA2841184C|2017-12-12|

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CA2984340A1|2013-02-07|

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US20130168257A1|2013-07-04|

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US20160207106A1|2016-07-21|

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US20130029886A1|2013-01-31|

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EP2737108A4|2015-08-05|

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EP2737108A2|2014-06-04|

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US10092953B2|2018-10-09|

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WO2013019409A3|2013-07-11|

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AP2014007389A0|2014-01-31|

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EP2737108B1|2019-08-21|

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DK2737108T3|2019-11-04|

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CN103703165B|2016-08-17|

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CA2841184A1|2013-02-07|

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CN103703165A|2014-04-02|

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US9643250B2|2017-05-09|

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CA2984340C|2021-06-01|

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WO2013019409A2|2013-02-07|

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AU2012290564B2|2017-02-16|

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MY169350A|2019-03-21|

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法律状态:
2018-04-03| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|

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2019-08-06| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|

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2020-06-30| B06A| Patent application procedure suspended [chapter 6.1 patent gazette]|

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2021-02-02| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|

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2021-04-27| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 18/07/2012, OBSERVADAS AS CONDICOES LEGAIS. |

优先权:

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申请号 | 申请日 | 专利标题

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US13/194,271|2011-07-29|

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US13/194,271|US9643250B2|2011-07-29|2011-07-29|Method of controlling the corrosion rate of alloy particles, alloy particle with controlled corrosion rate, and articles comprising the particle|

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PCT/US2012/047163|WO2013019409A2|2011-07-29|2012-07-18|Method of controlling the corrosion rate of alloy particles, alloy particle with controlled corrosion rate, and articles comprising the particle|

---