JPS62197141A - Production of synthetic material finely divided and alloyed - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention generally relates to synthetically processed materials. More particularly, the present invention provides a material in which at least one of the precursor components is synthesized from an energetic species and exhibits a range of mechanical, chemical, optical, thermal and electrical properties hitherto unobtainable in naturally occurring similar materials. The present invention relates to a method of manufacturing such a novel material.

The present invention is based on the growing worldwide need for materials with a range of properties not present in naturally occurring materials. In order to free ourselves from the constraints of natural materials, technological innovations that allow us to synthetically process materials with unique properties are essential. The purpose of the innovations described below is to provide thermal, electrical,
The aim is to overcome the constraints that until recently limited the effective range of optical, structural and chemical properties to a relatively narrow range. Breaking through the same constraints as naturally occurring materials allows the production of materials with non-stoichiometric compositions, unique electron orbital configurations, and mutant bonding. Such non-standard compositions and configurations can be used to synthesize new materials with infinite combinations of desired properties.

The main objective of the present invention is to provide a method for producing synthetic materials that are specially treated to suit any desired application. To achieve such a bold goal, it is necessary to introduce energetically excited component species into the host matrix of the base material in a novel manner. According to this novel manufacturing method, the synthesized electronic and chemical bonding configurations of the component species in the host matrix are altered and permanently maintained. In this text, the term "component" or "component material" refers to any species that participates in the interactions that lead to the final synthetic processed material, even if this species is physically present in the final product. It doesn't matter whether you say no or not. The components may particularly include inert scum or other species that transfer energy or otherwise influence the formation of the material.

Methods for the production of prior art synthetic materials characterized by a narrow range of chemical, optical, thermal, electrical and physical properties not present in naturally occurring materials have already been described in the literature on "quenching processes". ing.

When the precursor material is quenched from a non-solid state, nonequilibrium states and local bonding order characteristic of the state of the precursor material can be maintained in the quenched state. In contrast, when the same precursor material is slowly cooled from a non-solid state to a solid state, a material is formed that does not exhibit the non-equilibrium states and local bonding order possible with quenched materials. Typically, the nonequilibrium state produced by quenching includes at least some phases characterized by a disordered amorphous, microcrystalline or polycrystalline structure, optionally with crystalline inclusions. Because the properties of materials produced by quenching are different from those of slow-cooled materials, fast quenching can be used commercially to produce amorphous disordered materials in bulk and thin films that do not exhibit the desired novel properties.

To date, rapid quenching techniques have involved adding one or more "modifying" elements to a preselected material's host matrix (physical, chemical, thermal, electrical, or optical properties).
used to modify one or more of the sexes as preselected. This modification is desirably carried out without loss of other properties, but it is believed that these other properties of the naturally occurring or unmodified material will be correlated with and influenced by the modified properties. The principle of this modification according to the present invention will hereinafter be referred to as "modified WJ".In other words, in the present invention, the term "modification" refers to the introduction of a modifying species into the host matrix of the precursor material to Means to modify without correlation to properties.According to a preferred definition, modification will affect the post-7 trix electronic configuration, as described in detail below.

As mentioned above regarding high-speed quenching, the host material of the precursor material
It will be appreciated that a variety of other methods may be used to add modifying elements or species to the gas. for example,
Up until now, modified amorphous materials have been developed by, for example, thin film processing, C
It is manufactured by VD, sputtering and co-sputtering, glow discharge and microwave glow discharge. These modification methods, the modified materials obtained by these methods, and the unique properties obtained by the modification are known, for example, from SLanf
ordR.

Ovshinsky U.S. Pat. No. 41.77473 [
"Amorphous semiconductor materials and their manufacturing method", Stanfo
rd R. Ovsbinsky U.S. Patent No. 41.77
No. 474 “High-temperature amorphous semiconductor material and its manufacturing method”
, Stanford R. (lvsbinsky and K.
U.S. Patent No. 4,178,415 to Rishna Sapru
No. “Modified amorphous semiconductor material and its manufacturing method”, St.
anlord R.

Ovsbinsky and Masatsubu Tzu, U.S. Pat. No. 4,217,374, "Amorphous Semiconductor Equivalent to Crystalline Semiconductor Material Produced by Glow Discharge Process," Stanford R. Ovshinsky, U.S. Pat. No. 4,520,039, entitled "Materials with Variable Composition and Process for Making the Same."

The modified material described in that patent is formed of a solid amorphous post matrix with a structural arrangement having local order rather than long range order. Similarly, according to the principles disclosed in these patents, a modifying species having electron orbitals that interact with the electron orbitals of the host matrix of the precursor material may be added to the host matrix. As a result of this interaction, the electronic configuration of the post-matrix of the precursor material is substantially modified. It has an atomic arrangement that has been changed to give it an independently increased electrical conductivity. The resulting material exhibits both chemical and structural modification, with properties typical of non-equilibrium materials with modified local order, structure and configuration changes as a result of both modifications. can get.

Regarding the present invention, it is particularly important to describe the modification of the host matrix of the precursor material by the melt spinning process. This is 5tanford R.

0vsh 1nsky and Ric h a r d^
No. 4,339,255 to F1a5ck, entitled "Process and Apparatus for Making Modified Amorphous Glass Materials," which patent is assigned to the assignee of the present invention. The '255 patent describes a method and apparatus for introducing flow modifiers into a host matrix. The flow modifier includes one or more inert gases such as oxygen, nitrogen, silicon tetrafluoride or arsenic hydride. The synthetic material produced by the method described in the bulk patent may be a modified amorphous glass material of metal, dielectric or semiconductor. The range of modified synthetic materials extends from alloys, to materials with varying degrees of alloying and modification, to materials in which only modification and doping effects are present. The method described in U.S. Pat. No. 255 discloses modifying species that can be added in various intervals or layers at various rates and in various orders, but the number of species added, the number of layers, and the spacing, speed and order of introduction are limited.

Using the method described in US Pat. No. 4,339,255 it is even possible to produce modified ceramic materials, such as ceramic materials exhibiting properties that do not occur naturally in standard preparation materials. In addition, since the interaction between the modifying material and the precursor material forming the host matrix does not occur in the crucible that liquefies the material, but occurs on the surface of the spinning chill wheel, the resulting material has a composite structure. , a modulated structure or a layered structure.

Although the method described in U.S. Pat. No. 4,339,255 does not produce modified ceramic materials, the material obtained in this manner can be spun onto the peripheral surface of a chill wheel. As mentioned above, melt spinning is a rapid cooling method and has a high rapid cooling rate of 108° C. per second. However, as it currently stands, melt spinning is one of the slower quenching techniques, especially when compared to faster techniques such as sputtering, so it has not been possible to produce modified bulk materials at higher quench rate ranges until now. I couldn't. It is of course preferable (for the production and production of the highest quality modified material) to produce the modified bulk material at very high quench rates. Because of the limited quenching rate, the present invention
Concerning innovative manufacturing techniques for synthesizing new types of modified materials. This technology is described in F1a5ck's U.S. Patent '25.
It does not have any of the limitations of the method No. 5 and other quenching methods developed so far. More specifically, F1a5ck U.S. Patent No. '255
The method described in this issue has problems such as being able to produce only relatively thin film materials, forming only a small number (1, 2, or 3) of thin film material layers, or being limited to one type of hostra 1 to lyx precursor material for each layer. Has restrictions. Also, the method of US '255 does not disclose the use of a core member on which the modified thin film material is deposited.

Additionally, although U.S. Pat. No. 255 discloses the production of modified dielectric materials, the melt spinning process used therein has a fairly low rate of modification-like diffusion into the host matrix. It is not possible to produce highly effective classes of materials, such as classes of ceramic materials with properties modified at the atomic level, using the methods described in . They can exhibit combinations of properties not seen in exogenously produced ceramics.

In contrast to previously developed high-speed quenching methods such as those described above, the present invention utilizes liquefied metal, semiconductor or ceramic pos.
We provide a method for producing a synthetically processed material in which an energy-modifying element is introduced into 7 Trix. Since the manufacturing method of the present invention can be cycled using multiple types of host 7 trix materials, sequentially deposited layers of phos 1 to 7 trix may be repeatedly modified with the same modifier or with different host 7 trix materials. It may be sequentially modified with modifiers to form a multilayered bulk material with varying compositions, or a relatively thick, homogeneous single bulk material may be formed. Alternatively, the externally treated core member may be passed through a series of deposition stations to deposit the modified material onto the core member. Finally, the method of the present invention provides the necessary high concentration for the interaction of the precursor material's host molecules and the modified material to occur during exposure to the atmosphere and while the modified material is maintained in an active state. Both quenching speed and high diffusivity are obtained. The addition of energy-modifying species to the host polymer I-plus at high diffusivity allows the production of truly atomically h-gold ceramic materials.

The present invention provides a method for producing a synthetically processed solid material. The method includes the steps of: providing a flowing stream of a first component of material; acting on the flowing stream of the first component a second component of an excited diffusible material; and diffusing the second component. In this way, the second component interacts with the first component to form a synthetically processed solid material exhibiting a range of properties different from those of the individual components. The first component fluid stream is preferably liquid and substantially formed of a material selected from the group consisting of metallic materials, semiconductor materials, semi-metallic materials, ceramic materials and combinations thereof. Preferably, the excited gaseous material stream is guided to impinge on the flowing stream of the first component. The gaseous material consists essentially of nitrogen,
selected from the group consisting of oxygen, halogens, hydrocarbon gases, inert gases, hydrogen, vaporized alkali metals, and combinations thereof. The second component may form plasma, generate ions, become radicals, or be thermally activated.
It can be excited by photoactivating, catalytically activating, or by utilizing a high pressure environment.

The excited gas flow contacts the first component flow stream substantially in the direction of movement of the first component such that momentum is transferred from the gas flow to the first component flow stream. Contact of the two streams is maintained for a sufficient time to reach the desired degree of diffusion. In a preferred embodiment, the first component is digested in a crucible and expelled from the crucible as a fluid stream. The injection may be in the form of injection from a pressurized nozzle. In another embodiment, the first component may overflow from the top of the crucible. The opening formed in the crucible may be regular with a circular or square cross section, or irregular with a bow tie or I-beam cross section.

−． -48- Preferably, additional energy is applied to the flowing stream of the first component to promote diffusion of the second component in a portion of the post-matrix bulk of the first component. For this purpose, pulsed energy is applied to the flowing stream to generate eddy currents within it. The external energy may be provided as electrical energy, magnetic energy, mechanical energy, or optical energy. A flowing stream of an additional precursor component is directed into contact with a flowing stream of the first component. The third or additional component may be guided simultaneously or sequentially into contact with the first component, on a quenching surface to freeze the properties of the modified material after the components have interacted. can be used.

A core member may be used to deposit a layer of modified acid-treated bulk material. Plus to activate the second ingredient? AC energy, microwave energy, RF energy, or DC energy may be used to form the .

The present invention further discloses a method for producing relatively thick synthetically processed solid interest. The method includes disposing a core member (nu
directing the core member to at least one deposition station configured to provide a fluid stream of a first component of the synthetic process material; applying a second component of the possible material; and diffusing the second component into at least a portion of the flowing stream. In this way, the second component is brought into contact with the first component to deposit a layer of synthetically processed solid material on the core exhibiting a range of properties different from those of the individual components. The core is preferably formed from a material having a similar composition to that forming the acid treated solid material. Preferably, a plurality of deposition stations are provided and the cores are sequentially guided to the plurality of deposition stations. The fluid stream of the first component is preferably a liquid stream formed from an atomized metallic material, an atomized semiconductor material or an atomized ceramic material. The second component is brought into contact with the flowing stream of the first component by utilizing the excited gaseous material flow. The excited gaseous material is selected from the group consisting essentially of nitrogen, oxygen, halogens, hydrocarbon gases, inert gases, hydrogen, vaporized alkali metals, and combinations thereof.

The second component is excited by plasma, ionization, radicalization, thermal activation, photoactivation, catalytic activation or the use of a high pressure environment. The core member is specifically configured to function as a mold to which successive layers of synthetically processed solid material are deposited. The excited gas flow collides with the first component flow stream and is guided such that the momentum of the gas flow is transferred into the first component flow stream. The first and second components are highly diffused. Maintain contact for a sufficient period of time to obtain a degree of

Preferably, the first component is liquefied in the crucible and expelled from the crucible as a fluid stream. The first component may also be injected from the crucible via a pressurized nozzle or may overflow from the crucible. Moreover, the opening of the crucible may be either regular or irregular. However, in this embodiment, the sequentially deposited layers of synthetic processing material need to be injected through an aperture shaped to produce a product of a predetermined final cross-sectional shape.

An Energ A-burst may be applied to the flow stream of the first component to promote diffusion of the second component in the first component Pos I-Ma I-Plus. The energy may be electromagnetic or thermal energy, or may be supplied, for example, from eddy currents or any other source of energy that produces (for example) agitation of the first stream. Excited diffusible 3rd, 4th and 5th components of the synthetic treatment material may be used, in which case excited diffusible (for example) 2nd. Third. The fourth and fifth components are allowed to act on the first component prior to quenching. After interaction with this second component and additional components, the modified material may be deposited on a quenched surface to freeze properties in the material.

The synthetically processed solid material may be formed as elongated fibers that can be collected on a take-up spool. The take-up spool may exert a biasing force along the longitudinal direction of travel of the fibers to facilitate passage of the fibers through multiple tUa stations.

The present invention further provides a novel method for manufacturing optical transmission fibers.

The method includes the steps of providing a flowing stream of a first component selected from one or more Group I elements and applying excited oxygen to the flowing stream.

The excited oxygen then diffuses into at least a portion of the flowing stream.

In this way, the oxygen interacts with the first component to form a synthetically processed light transmission fiber. The first component of the fluid stream is selected from the group consisting essentially of silicon, germanium, and compounds, combinations and mixtures thereof. This fluid stream also contains additional polyvalent metals. The method may further include applying an excited third component to the fluid stream. The third component substantially includes one or more elements selected from halogens, polyvalent metals, nitrogen, and alkali metals.

Also disclosed is a method for producing a synthetically processed solid material. The method includes the steps of: providing a moving surface; contacting at least a portion of the moving surface with a flowable first component of the material; and contacting a portion of the first component of the moving surface with a flowable second component of the material. and catalytically introducing an excited third component of material T1. This material consists essentially of (1) a first component, (2) a second component,
(3) configured to diffuse into a component selected from the group consisting of the first component and the second component; As the third component diffuses and catalytically interacts with the selected components, a synthetically processed solid material is formed which exhibits a range of properties different from those of the individual components.

The moving surface may be in the form of a moving belt, for example, or the surface of a drum or rotating wheel.

One or both of the flowable first and second components may be melted to form part of the fluid stream that is injected from the crucible. Alternatively, one or both of the flowable first and second components may be provided as an immersion bath or a spray, such as a plasma spray. Alternatively, multiple moving surfaces may be deployed in a multilayer deposition step process.

The excited third component may be catalytically introduced to diffuse into the first component during or after contacting the first component with a portion of the moving surface. Alternatively, an excited third component may be catalytically introduced into the second component prior to or during contact of the fluid second component with a portion of the first component of the moving surface. Alternatively, the excited third component may be catalytically introduced into the backbone after mutual contact of the fluid first and second components.

According to another embodiment of the invention, a synthetically processed composite material is prepared. The synthesized composite material sequentially includes a micron or submicron scale ceramic zone, an inner zone of a different composition, and a ceramic seam.

In the preparation of synthetically processed composite materials, at least two
Forming a body containing different types of materials. The materials include a relatively reactive first material and a relatively non-reactive second material. For example, the body can be gas sprayed, sprayed onto Mel 1, melt spinning, sputtering, CVD, plasma CVD,
It can be prepared by rapid solidification techniques that produce fine microscopic structures, such as microwave-excited plasma CVD.

After formation of the microscopic body, the body is contacted with a highly excited reactant, such as an oxidizing agent.

The reactants may be gaseous reactants, such as nitrogen or oxygen, or solid reactants such as carbon, which are highly excited. The excitation may be microwave radiation, ion beam excitation, thermal excitation, or electrical excitation.

When the excited reactant contacts the body, a relatively reactive first
The material reacts with the reactants to form micron-scale ceramic zones. At the same time, probably Cabrara-M
As a result of ott diffusion, a zone of concentrated relatively non-reactive material is formed.

Relatively reactive materials and relatively unreactive materials have different rates of reaction with oxidizing agents. For example, at the same temperature and nitrogen activity, a relatively unreactive metallic material will have a slower nitridation rate than a relatively reactive material; at the same temperature and oxygen activity, a relatively unreactive metallic material will The oxidation reaction rate is slower than a relatively reactive material, and when the oxidizing agent is carbon, a relatively unreactive metal material at the same temperature and carbon activity has a carbonization reaction rate slower than a relatively reactive material. .

Relatively reactive materials are Ti, J Cr, Zr, N
b, Mo, Hf, Ta, IA, layer, Y, M, and Si. The relatively non-reactive metallic material is selected from the group consisting of Fe, Co, and Co.

The resulting synthetically processed composite material is flakes, chips,
It may have the form of a powder, filament, wire or ribbon.

The material can be manufactured into various forms. For example, it may be pelletized by containing carbon.

To this end, dispersed particulate carbon is added to a solid alloy and the carbon-containing alloy is pelletized to form a solid carbide-containing cermet.

Alternatively, particulate materials such as powdered materials, filamentary materials or acicular materials may be formed as mats or bodies in the composite material and bonded by a binder such as a polymer or molten metal. Thus, according to another embodiment of the invention, a web of substantially filamentary material may be formed. The web may be contacted with a molten metal binder and then cooled to form a bonded composite.

Other objects and advantages of the invention are fully explained by the claims, written description, and accompanying drawings.

The method of the present invention will be more fully understood from the following detailed description based on the accompanying drawings. In FIG. 1, the entire deposition station is designated by the reference numeral 1. This deposition station is designed to produce synthetically processed materials. More specifically, the deposition station 1 contains a crucible 3 in which a first component of the precursor material (forming phosphorus) is liquefied, for example by induction heating 17, to form a liquefied first component. 2 and is released from the opening 5 at the bottom of the crucible. The liquefied first component 2 is then transformed into a liquid KL.
7, and this flow stream forms a regular or irregular opening 5.
ejected from. The deposition station 1 also incorporates a nozzle 9 from which the excited diffusible second component of the material to be synthesized is ejected and the second component of the material to be processed is ejected.
A stream 11 is formed in which the components can easily diffuse. As discussed in more detail below, it is important that the second component be introduced into the flowing stream of the first component in a highly active state.

According to one embodiment of the invention, the first component of the synthetic treatment material is melted in the crucible 3. This first component is, for example, a metal, an r-conductor or a ceramic material.

Melting can be done using resistance heating, induction heating, or other techniques that do not add impurities to the liquefied material. In some cases, the first component is normally liquid and therefore there is little or no need to apply external heating. Irrespective of the room temperature, the first component 2 dissolved in the liquid 1 is released from the crucible 3 through the opening 5 and emitted from there. Form l f4 flow stream 7. Note that the first component is a material with a lower melting point than the crucible making material. This is an essential requirement to prevent contamination of the liquid stream by impurities introduced into the crucible 3.

The flowing stream 7 of the first component of the synthetic treatment material is then acted upon by the excited second component of this treatment material. Excitation of the second component is performed by inputting electrical, optical, magnetic, photochemical, chemical or thermal energy. For example, the second component may be exposed to an electromagnetic energy field such as a microwave, R, F, wave or other alternating electric field. Similarly, an excited plasma may be formed by being excited by a DC electric field. The excitation may be optical excitation, for example by irradiating the component with light of a suitable wavelength to generate an excited species from the component. Thermal energy may also be used to generate the excited species from the second species. In some cases, catalyst activation may be used. For example, molecular hydrogen gas may be contacted with platinum or other catalytic material to produce excited atomic hydrogen. More detailed explanations and descriptions of various excitation structures will be described in detail below with reference to FIGS. 78 to 7D. In order to facilitate the explanation of the inventive step, it is assumed that the activation occurs inside the nozzle 9 and that the excited species are ejected from the nozzle 9.

Regardless of the method used, excitation of the second component generates ions, radicals, molecular fragments and/or stimulated neutral species from the second component. In the text, the term ``excited species'' refers to an atom, molecule or fragment thereof with increased reactivity, regardless of how the increase is effected.Furthermore, the second component is , may be exposed to activated energy or catalytic material at a location remote from or within the nozzle 9. For example, electromagnetic energy may be incorporated into the structure of the nozzle 9, such as an electrode, waveguide or spark gap. An important feature of activation is that the species is maintained in an excited state until downstream diffusion of the second component with the bostomatoid matrix is complete.

The excited diffusible second component is ejected from the nozzle 9 in close proximity to the fluid stream 7 emerging from the crucible 3 and forms an activated region, e.g. a bladder of activated species 11, which substantially surrounds the fluid stream 7. ? form. Since the second component is in the activated state and the first component is in the molten state, the second component easily diffuses and interacts with the flowing stream 7, resulting in properties that differ from those of either component when cooled. A synthetically processed solid material with a range of properties is formed.

As shown in FIG. 1, the deposition apparatus is housed in a chamber 4. This chamber is not necessary for all manufacturing methods. However, in many cases it is desirable to produce certain synthetically processed materials in a controlled environment. For example, chamber 4 is filled with an inert gas, such as argon, to shield the fluid stream from environmental contamination. In another example, chamber 4 may be evacuated via pressure line 4a for the same purpose. In yet another example, the treatment may be performed at elevated temperatures in a pressurized atmosphere to facilitate reaction and/or diffusion of the components. Of course, at elevated room temperatures the first component will remain in a liquid state for a longer period of time.

According to another preferred embodiment shown in FIG. 2, the liquefied first component of the treated material is ejected from the nozzle 6.

The nozzle forms part of the crucible 3 and substantially surrounds an opening 5 formed in the bottom of the crucible. The fluid stream 7 is injected from the crucible 3 via this nozzle 6. Optionally, a fluid stream 7 may be discharged from the pressurized crucible. In the embodiment of FIG. 2, r, f, spaced electrodes 8a coupled to an energy source.
, 8b imparts a burst of energy to the flowing stream 7 discharged from the crucible 3. or at a location downstream of the flowing stream 7 emitted from the nozzle 6 .
An r, f wave induction coil 8c (indicated by a dotted line) shaped to substantially surround the wave induction coil 8c may also be used. Spaced electrodes or induction coils provide additional energy to promote reactivity and diffusion of the second component to the first component of the synthetic treatment material. Additionally, induction coils or spaced electrodes may be used to generate eddy currents within the flowing stream. The eddy currents function to agitate or mix the molten material, maintaining its reactivity and promoting homogeneous reaction with the second component. In another embodiment, eddy currents may be generated by the action of a magnetic field applied across the flowing stream 7. The motion of the flow stream and/or the motion of the magnets generates the necessary forces to initiate and maintain the eddy currents.

In some instances, it may be desirable to provide additional electrodes (not shown) in the vicinity of the melt stream 7 to facilitate the transfer of selected ions of the activated second component into the flowing stream. In some cases, the material forming the flowing stream 7 will have a sufficiently high electrical conductivity that it can be directly biased to promote ion migration. The flowing stream then constitutes an electrolyte that receives ions. Regardless of the method of supplying the additional energy, the excited diffusible second component of the treatment material is ejected simultaneously from the nozzle 9 described with respect to FIG. A synthetic treatment material body is formed under the action of diffusion effects.

According to a preferred embodiment of the invention shown in FIG. 2, a molten first component 2 of the material to be treated is ejected from the crucible 3 via a pressurized nozzle 6 to form a fluid stream 7. r, f, output electrodes 8a, 8
The energy pulses emanating from b generate eddy currents in the flowing stream 7 as described above. In this way, the flow stream 7 is
It is maintained in an excited state during exposure to a plasma 11 formed from the excited diffusible second component of the treatment material. Eddy currents in the flow stream 7 cause excited diffusible secondary
Promote faster diffusion of ingredients and ensure more uniform and homogeneous modification of post materials. Moreover, the iMed three-component solid materials exhibit a correspondingly improved homogeneity and uniformity with respect to material properties.

Another preferred embodiment of the invention is shown in FIG. In FIG. 3 a first nozzle 9a is shown which emits an excited stream of an excited diffusible second component of the treatment material. Furthermore, in contrast to FIGS. 1 and 2, a second nozzle 9b is shown which emits an energized flow stream of an energized diffusible third component of the treatment material. In operation, a fluid stream 7 of the first component injected from the crucible 3 is formed as described above and discharged through regular or irregularly shaped openings 5.

After this ejection, said flowing stream contacts a plasma llu formed from the excited second component and a plasma llb formed from the excited diffusible third component, leading to the diffusion and interaction of both the second and third components. The action forms a synthetically processed solid material that has been modified. Although only two types of diffusible modifiers are illustrated, it is understood that an additional nozzle could be provided to provide additional excited modifiers to the flow stream formed by the first component. It will be. In some examples, additional nozzles may be used to provide unexcited components to the flowing stream for interaction with, heating, cooling, or modifying the material being produced. If the second component is sufficiently reactive, it may be chemically excited by contacting it with the flowing stream 7, in which case no external activation or excitation is required.

It will further be appreciated that in the particularly preferred embodiment shown, the flowing stream 7 receives the action of the second and third components in sequence. However, in another particularly preferred embodiment, the excited second and third components act simultaneously on the flow stream. The desired modification to be carried out in the final external material, whether by simultaneous or sequential interaction of the components;
Selection is made by composition gradient, degree of doping or alloying.

FIG. 48 shows yet another preferred embodiment of the present invention.

This embodiment includes a quench surface for rapid solidification of synthetically processed materials. The apparatus of FIG. 4Δ includes a crucible 3;
is almost the same as crucible 3 in the previous specific example. As shown, the crucible 3 is equipped with an induction heating coil 17 for melting the first component 2 of the treated material contained therein. Other non-contaminating heating methods may also be used, such as resistive heating or radiant heating as described above.

Also provided is a nozzle 9 which is almost the same as the nozzle shown in the previous figures, and this nozzle 9 is used for treating the material 1 in a plasma state.
J1 is configured to emit and excite the diffusible second component of J1.
has been done. The nozzle 9 in FIG. 4A (indicated by dotted lines IJ-) injects the second component either at a location near the surface of the wheel 21 or at a location B remote from the surface of this wheel. The location where the second component interacts with the first component stream 7 determines the degree of diffusion.

The difference between the previous apparatus and the apparatus of FIG. 4A is the provision of a chill wheel 21 for high speed quenching of the reformate stream within the permanently treated material. Typically, the chill wheel 21 is formed from a material with high thermal conductivity, such as copper or aluminum, and rotates at high speed to aid in lifting and cooling the material during the material manufacturing process.

According to FIG. 4A, a flowing stream 7 of the first component of the treatment material is guided from the crucible 3 to the peripheral surface of the chill wheel 21. According to FIG.

The first component stream 7 is acted upon by an excited second component of the material to be treated. In one embodiment, the second component is injected from the nozzle 9 at a location substantially aligned with the location where the first component is introduced into the chill wheel 21 . The second component diffuses into and interacts with the first component to produce a synthetic treated material. This material rapidly solidifies by conduction of heat from the chill wheel 21. Furthermore, the rotational force of the wheel serves to quickly separate the prepared treatment material body from the peripheral surface 24 of the chill wheel 21. In the second embodiment of FIG. 4Δ, the second component plasma 11 interacts with the first component at a location (position B) spaced from the location where the first component is introduced into the chill wheel.

■Refer to Figure 4B for the response from ゞ'ζ or jet. FIG. 4B shows an apparatus suitable for another preferred embodiment of the invention. The apparatus of FIG. 4B is substantially similar to the apparatus of FIG. 4B, and like elements are designated by the same reference numerals. The differences in the apparatus of FIG. 4B compared to the apparatus of FIG. 48 include the introduction of additional components into the synthetically processed material body during its manufacture and the provision of wheels with one or more quenching surfaces. This is what is being done.

The device of FIG. 4B includes a wheel 21 and an induction heating coil 17.
A rattling crucible 3 and a first nozzle 9 are installed. These elements are substantially similar to those described with respect to FIG. 48 and need not be described. The apparatus of FIG. 4B further includes a container, such as a barrel I.18, that holds a bath of liquefied material 20. As shown, vat 18 includes a resistive heating element 22 that maintains the temperature of liquefied material 20 . The device further includes an induction coil 19
1), including a second nozzle 9b coupled to an energy source such as 1). The second nozzle 9b is substantially similar to the first nozzle 9LI and is configured to apply a reforming material to the liquefied material stream or body 7.

The function of the apparatus of FIG. 4B will be described with respect to the preparation of a typical synthetic process material, in this case a silicon glass member doped with tin and zirconium.

In preparation for the treatment, the crucible 3 is first filled with high purity silicon, and the induction coil 17 is excited to melt the filled silicon 2. The first nozzle 9a is configured to provide a flow of excited oxygen and the second nozzle 9b is configured to provide a flow of excited hydrogen. The wheel 21 has a peripheral contact surface made of zirconium or coated with zirconium. The vat 18 is filled with tin tetrachloride 20.

During operation, the wheel 21 is filled with tin tetrachloride 20 rose I.18
, and traps a stream of tin-containing material on its surface 24 during this passage. The molten silicon is injected from the opening 5 in the bottom of the crucible 3 into a flowing stream 7 and reaches the peripheral surface 24 of the wheel 21. This molten silicon stream 7 interacts with both the zirconium wheel surface 24 and the tin tetrachloride present thereon, and these materials are added to the host matrix of silicon compounds to alloy the host matrix.
Doping and/or modification is achieved. The molten silicon in which tin tetrachloride and zirconium are mixed in 7trix is subjected to the action of excited oxygen plasma lla from the first nozzle 9a, and this oxygen converts the silicon into silicon dioxide containing zirconium and tin tetrachloride. The silicon dioxide body thus formed is then (once said addition is completed) subjected to the action of an excited hydrogen plasma 111J emitted from the second nozzle 9b. This hydrogen diffuses into the silicon dioxide body and reduces tin tetrachloride 72-1 to liberate tin. In this way, silicon dioxide containing zirconium and tin is prepared.

It will be apparent to those skilled in the art that modifications may be made to the invention without departing from the spirit and scope of the invention.

For example, instead of tin tetrachloride, molten tin could be supplied to the bud 18, in which case energization of the heating element 22 would be required to maintain the tin in a liquid state.

In such embodiments, the use of activated hydrogen to reduce the tin tetrachloride is not necessary. In another variant embodiment of this method, the peripheral surface 24 of the plug 21 is formed from or coated with tin, and the butt 18 contains a zirconium-based material, such as a zirconium halide. . In yet another embodiment, vat 18 and/or wheel 21 are maintained at an elevated temperature to facilitate reaction of the components to be combined to form the composite treated material. Furthermore, as described above, the positions of nozzle 9a and nozzle 911 may be changed to modify the material produced.

The method described with respect to FIG. 4B can be easily applied to the manufacture of many materials other than silicon dioxide-based materials. Additionally, the basic process shown in Figure 4B can be expanded or simplified to meet various requirements. For example, butt 18 may be omitted and the introduction of the components to be combined to form the body of treated material may depend on the surface of the wheel.

or the wheel 21 is rendered inert to the process;
Component introduction may depend solely on the vat 18.

In some cases, surface 24 of wheel 21 may not provide one component of the body being manufactured, but may be formed to function as a catalytic surface to facilitate interaction of the components. For example, wheel surface 24 may be formed from iron, precious metals, ceramics, cermets, or another catalytic material particularly suited to promoting interaction. Furthermore, the apparatus of FIG. 4B can also be used without crucible 3. In such embodiments, the wheel 21 can provide a sufficient flow of the first component 20 from the vat 18, which is then acted upon by the second and subsequent components from the nozzles 9a and 9b. Additionally, the apparatus of Figure 4B may be modified to include additional nozzles that supply additional components of the processing material.

According to another variant embodiment, the quench wheel may be replaced by a moving surface, such as a belt, a drum or one or more rollers. Multiple moving surfaces may be provided to synthesize multilayer materials. Spurs may be used to provide a flow component that contacts a portion of the moving surface.

Figure 5 shows an apparatus consisting of a plurality of deposition stations operatively arranged to produce thick bodies of synthetically processed solid materials. The device comprises a first crucible 3, similar to the crucible described in the ordinary light, associated with the crucible 3 at least one nozzle 9 for emitting an excited modifying component. The apparatus also includes a second crucible 2 operatively located downstream of the first crucible 3.
Also associated with the crucible 23 is at least one second nozzle 29 . As shown by the dashed line,
The apparatus may further include any number of deposition stations associated with the apparatus. As shown, the last station includes a third crucible 33 operatively located downstream of the second crucible 23, with at least one third nozzle 39 associated with the crucible 33. .

The apparatus shown in FIG. 5 has been found to be particularly advantageous when large bodies of treated material are to be produced by successive deposition of thin film layers of said material.

A device such as that shown in FIG. 5 can also be used for e.g.
It is very useful in the production of multi-Nj structures containing thin film layers of different compositions, such as alloy compositions or DO-11 compositions. The operation of this device is an extension of the principles described for the components 76 above, and therefore the various modifications made with respect to the components described above may also be applied to the device of FIG.

In operation, the first crucible 3 is charged with the first component of the material to be treated and heated by the coil 17, emitting a liquid stream 7a from a specially shaped opening 5a provided in the bottom of the crucible 3. As in the embodiments above, the liquid stream of the first component is exposed to a plasma lla of an excited diffusible second component emitted from the first nozzle 9 of the treatment material.

The second component diffuses into and interacts with the liquid stream 7a, thereby forming the body of the synthetic treatment material.

The process material body formed at the first deposition station serves as the first core material for the successive deposition of thin film layers at downstream stations of the apparatus. As shown in FIG. 5, the body of treated material, hereinafter referred to as core, passes through a second crucible 23 loaded with the first component. that the core has been modified by interaction with the second component into a material having a higher melting point than the first component and therefore passes through the molten body in the second crucible 23 without liquefaction or deterioration; It should be pointed out that getting.

A liquid stream 7b of the first component loaded into the crucible 23 is deposited around the core as it exits the second crucible 23. This liquid stream 7b interacts with a plasma 1.1b consisting of a second component emanating from a second nozzle 29 of treatment material, so that an additional layer 7b of treatment material is deposited around the core. .

It is thus clear that relatively large bodies of synthetically processed material can be formed by successively repeating the steps described above. This is also shown with respect to the last crucible 33 of the apparatus of FIG.
C interacts with the excited second component plasma 1.1c to deposit a final layer 7C around the multilayer core ejected from the crucible.

As the body of the material being processed increases, nozzles are operationally associated with the crucible in successively arranged downstream deposition stations to completely surround the liquid stream with a sufficient amount of the excited second component. It should be noted that it may be necessary to Although the foregoing discussion of FIG. 5 pertains to a body of synthetic processed material that is substantially uniform in overall composition and is formed using the same first and second components in each crucible and nozzle. Obviously, the manufacturing method using the apparatus shown in FIG. 5 can be modified to produce successively a plurality of deposited layers of different compositions. For example, the core that has passed through the first crucible 3 is
A second crucible 23 containing a different molten material than that present therein can be fed. In this way, multilayer heterogeneous structures can be produced.

It should be pointed out here that the cross-sectional shape of the opening 5 provided in the crucible controls the cross-sectional dimensions of the synthetic treatment material body discharged from the crucible. According to the above, bodies with various cross-sectional shapes can be manufactured.

In some cases it is desirable to obtain a body with a substantially regular cross-sectional shape, such as circular, rectangular or elliptical, and it may also be desirable to obtain a body with a substantially regular cross-sectional shape, such as a circular, rectangular or elliptical shape, or a beam-shaped body to increase the catalytic activity, increase the surface area, or increase the surface strength. In some cases, it may be desirable to obtain a body endowed with a substantially irregular cross-sectional shape, such as. It should be noted that in order to achieve regular or irregular shapes as described above, only the first crucible 3 needs to have an opening 5 with a particular cross-sectional shape. In a plurality of subsequent stations, the core produced in the first chamber serves as a mold for subsequent layers deposited on the core, so that a large body with the desired cross-sectional shape is produced.

FIG. 6 shows a cross-section of a synthetic treated material body having an irregular cross-sectional shape selected for increased strength. From this figure, it can be seen that the external dimensions of the body are increased by successive deposition of deposited layers. The composite material body 40 shown in FIG. 6 has a generally bowtie-shaped cross-sectional shape (similar to an I-beam) and includes a plurality of successive deposited layers 41 a - 41 c surrounding a core layer 43 . The various layers 41a to 41c that cooperate with the core layer 43 to constitute the body may be formed with the same composition or may be formed with different compositions.

In some cases, a layer of a relatively hard material and a lubricious or flexible material are used to obtain a composite body of synthetically treated materials exhibiting advantageous but dissimilar) hardness, visibility and lubricity properties. It may be desirable to alternate with layers of. By controlling the amount of diffusion, it is also possible to deposit graded composition layers, said layers varying from a highly metallic composition to a highly ceramic composition.

Generally applicable to all of the figures above, the mass of the liquid flow of the first component of the treatment material f1 is smaller than the mass of the composite treatment body of said material 71, since the perfusion of the first component has a second component. Note that this is because body is obtained by adding ingredients. According to the law of conservation of momentum, the above factors must be accounted for in the motion of the liquid flow. first·
The liquid stream of the component is discharged from the crucible 3 and interacts with the second component as shown in FIG. be heavier (have greater mass) than the flow. ), the synthetic material body tends to move slower than the liquid flow (this is true since the river 1v1 must be equal to m2v2), this state of affairs is given by
This may cause splashing, agglomeration, agglomeration, or other uneven flow of the primary liquid stream.

To overcome the deleterious consequences described above, additional momentum must be imparted to the composite material body as it exits the deposition station. This can be realized in various ways. One highly preferred method (as mentioned above) is to introduce the second component of the treatment material through the nozzle at a velocity and at an appropriate angle sufficient to impart additional momentum to the flow of synthetic material. It would probably be sprayed from. This method can be accomplished relatively easily by angling the nozzle with respect to the liquid stream exiting the crucible. In other cases, the synthetic process material stream is from a deposition station;
Like a take-up reel (as shown in Figures 7A-7D) it is pulled onto a drum. By controlling the speed and torque of the drum J, sufficient momentum can be imparted to the flow to avoid the aforementioned flow problems. If a rapidly rotating chill wheel, such as that shown in FIG. 4A, is used, the wheel may also perform the function of imparting momentum to the flow to avoid the above problem.

The apparatus described with reference to the figures can be used advantageously for the production of a wide variety of synthetically processed materials.

This apparatus is particularly used for preparing higher temperature melting compounds such as ceramics and glasses from lower temperature melting components such as metals, semiconductors, etc. For example, the apparatus of the invention can be used to produce alumina bodies from aluminum metal and oxygen, or alternatively to produce Decnia bodies from datum. Aluminum nitride and titanium nitride are also prepared 46 by controlling the amount of diffusion. Additionally, interesting composite materials such as aluminum-alumina materials, titanium-titania materials or zircon-zirconia materials (and many other materials) can be produced. The above materials have many potential uses as reinforcing fibers, heat resistant materials, conductive ceramic type materials, etc. Those skilled in the art in the field of materials science have described the methods disclosed herein for producing homogeneous compositional and multilayered composites with uniform optical, electrical, mechanical, thermal and structural properties. It is anticipated that it will be readily adaptable to the preparation of synthetically processed materials of a wide variety of compositions.

2. Boume Tsuba Ran i Shinko As previously mentioned, various types of energy may be used in accordance with the principles of the present invention to activate the various energetic gaseous components of the materials to be synthesized. Some such excitation methods are illustrated in Figures 7A-7D.

FIG. 7A shows an apparatus generally similar to that of FIG. 1, which includes a crucible 3 heated by an induction coil 17 configured to prepare fibers 7 of synthetic process material.

Also shown in FIG. 7A is a winding wheel 60 configured to wind up and collect the fibers 7, this figure primarily showing that microwaves are used to excite the constituents of the treated material emanating from the nozzles 9a and 9b. It is intended to show the cases in which

For microwave use, the device includes a pair of microwave horns 62a and 62b located at a distance from each other, these horns 62a and 62b absorbing the scum-like reactive components emanating from the two nozzles 9a and 9b. is arranged to direct the microwave energy towards the flow of water. Microwave horns 62a and 62b are typical microwave sources or are otherwise known as "Woods horns" well known in the art.
r n s )”.

Naturally, the pawn is operatively connected to a microwave energy source (not shown). One particularly advantageous aspect is achieved by using a microwave horn,
This is because the highly active rays emitted from the horn activate far more species than with r, f, energy.

The gaseous components leaving the nozzles 9a and 9b pass through a field of microwave energy to form a plasma 11 from them.
The resulting plasma 11 interacts with the primary component of the liquid stream 7 ejected from the crucible 3.

As shown, the apparatus comprises a pair of r, f as previously described.
, also includes excitation electrodes 8a and 8b, which impart an additional energy to the fibers 7 in order to maintain an optimum temperature of the liquid stream and also to promote interaction of the components of the liquid stream. - It is arranged to do so.

FIG. 7B shows an apparatus generally similar in function and structure to that of FIG. 7A, but in this example the excitation of the gaseous components of the process material is controlled by the flow of gaseous components emitted from nozzles 9a and 9b. A pair of r placed nearby for effective operation
, f, excited type fi64a and 641). As in the case of the specific example using microwave energy, r
, f, the energy excites the gaseous component to generate plasma 11 from the component, and the generated energetic plasma 11
promotes the interaction of the gaseous component with the host matrix of the first component.

FIG. 7C shows an apparatus for thermally activating gaseous components of processing materials. As shown, two nozzles 9a and 9
Associated with each is a coiled resistive heating element 66 which imparts thermal energy to the gaseous components emitted from the nozzles 9a and 9b.

Although not shown, the nozzles 9a and 9b may also be modified to contain a catalyst mass, such as a platinum or palladium mass, for catalytically activating the gas passing through the nozzles 9a and 9b.

Figure 7D shows a device suitable for photochemical activation of gaseous components provided by nozzles 9a and 9b. The apparatus includes a pair of light sources 68 operatively arranged to illuminate the components emitted from the nozzles 9a and 9b. Light source 68 most typically provides a high intensity wavelength suitable for component activation. As the light source 68, known photochemical light sources such as mercury vapor vapor, sodium lamps, arc lamps, and lasers can be used.

88 = ■, Quality L"1" Figure 8 is a perspective view showing one of the mass production plans 1 to 1 through which the inventive concept of the present invention is realized, as currently presented by the applicant of the present invention.In Figure 9, The reactor assembly, designated generally by the reference numeral 70, includes a reaction vessel 72, which includes a reaction vessel 72.
Within, the synthesis of atomically processed materials takes place. Large container 72 includes a crucible (not shown) disposed within housing 73 that is heated by induction coil 17 . The components of the material to be produced within the reaction vessel 72 are activated in this example by microwave energy provided by microwave bones 62a and 62b located spaced apart from each other, said horns 62a and 62b respectively It is effectively connected to power supplies 63a and 63b for operation. Pressurized tanks 75a, 75b, 7 for processing materials
The gaseous components delivered from one or more of Convert to insertion I\. The energy is also useful for maintaining the first component liquid stream 7 released from the crucible in an active state;
Note that as a result, interaction between two or more components is promoted.

The entire reaction vessel 72 is heated or cooled by a temperature control coil 76. Reaction vessel 72 may also be pressurized or depressurized via pressure conduit 77, depending on the properties of the material to be treated.

■、- Top ゛Learning, excellent production゛The principle of the present invention is not only the preparation of modified ceramic materials ↑°1, which are normally allowed, but also the preparation of fiber optic materials 1''
It should be pointed out that it is also particularly advantageous for the preparation of +. Both of the two types of synthetically treated materials r1 described in - correspond to the above-mentioned definition of atomic ceramic material.

As is well known to those skilled in the field of fiber optics, the current technology for manufacturing fiber optic elements is a well-developed multi-step process, and the key steps of this process are
It has remained virtually unchanged since its inception. Typically, preform members are manufactured by solidifying a high purity starting material with a carefully selected refractive index into the desired rod shape. The manufactured preform member is heated to its softening point and drawn into fine fibers. Following the drawing process, the fiber is typically processed by: (1) altering the refractive index of the outer layer of the fiber; (2) tempering the outer surface of the fiber;
or cured and/or (3) treated to coat the fiber with a protective coating.

At least this manufacturing method produces fibers that are characterized by low optical loss? H is a cumbersome method that requires strict control of all parameters. Typical preforms have lengths of 6 inches or less, and the stretching process described above results in fibers that are 1 kilometer or less long.

It would clearly be desirable to eliminate paraple processing as described above. By using the principles of the present invention)
With this, it is possible to manufacture long fiber optic elements in a continuous process. Typical fiber optic elm I.
It includes a core, a cladding layer on the core, and a protective outer layer. The core is a light transmitting element and is therefore formed from a material that is highly transparent with respect to the wavelength of the light to be transmitted. Core materials of silicon oxide, germanium oxide, zircon oxide, and other similar oxides are used alone or in combination for the transmission of light in the visible and near-infrared regions.

The cladding consists of a material that is compatible with, but has a different refractive index than the core material. The refractive index of the core and cladding limits the transmission of light through the core-cladding interface, so that the transmitted light is confined to the core region of the fiber by total internal internal reflection. selected. The parameters for selecting the refractive indices of the two materials are well developed and known to those skilled in the optical fiber art. To prevent light from escaping the core, the core must typically have a higher refractive index than the cladding layer. Often, the core and cladding layers are made from the same material, such as silicon dioxide, while the core is made from polyvalent materials such as tantalum, tin, niobium, zircon, aluminum, lanthanum, germanium, or boron oxides. The refractive index is increased by the addition of metal oxides.

The cladding layer not only exhibits an appropriate refractive index with respect to the core, but also contributes to improving the durability of the fiber. For this purpose, the cladding layer may have one or more (=1) additional elements increasing the strength and limiting the transparency of the layer. Said elements increasing the durability may be present throughout the thickness of the cladding layer or Alternatively, it can be added only to the outer surface.Such durability-enhancing elements can be selected from carbon, nitrogen or fluorine, for example, when the cladding layer consists of a material based on silicon or germanium oxide.

In some cases, it is desirable to change the refractive index of the core so that no light exits the center of the core.

When such a core with a refractive index gradient is used,
Before the light reaches the interface with the crat layer, it is already efficiently and smoothly directed towards the center of the fiber. The refractive index gradient may be continuous or alternatively step-like. The use of such fibers with a refractive index gradient is also known to those skilled in the art.

Traditionally, the production of fibers with refractive index gradients has required tight control of the gradient curve, which is difficult to achieve in the preform manufacturing process.

However, by using the principles of the present invention, the above
; such a refractive index gradient is precisely and easily achieved by controlling the diffusion of the refractive index-altering material into the phos I.7 matrix of the fiber.

In most cases, fiber optic engineering (1) eliminates the leakage of light into the fiber, which causes crosstalk in communication systems, and (2)
) Furthermore, an encapsulating protective layer is provided further outside the cladding layer to increase the strength and integrity of the fiber. Such a dense layer is typically a relatively thick, durable layer of vitreous, ceramic, or other durable material.

There are a large number of fiber optics currently in use and research. The present invention provides (1) the preparation of ceramics, glass, and other inorganic materials that melt at relatively high temperatures through processes that eliminate major sources of contamination; (2) tighter control of the composition of the concentric layers; 3) greater control over the refractive index, and (4) improved control over all other physical properties of the material. will be apparent to those skilled in the art of device design and manufacturing. Additionally, the present invention can be used to produce very long fibers including fiber optic cores, crunds, and protective layers in a continuous single step.

For example, optical fibers may be fabricated in accordance with the principles of the present invention in an apparatus generally similar to that shown and described in FIG. It can be manufactured by In this way, fibers of high-purity silicon dioxide material are
It can be manufactured by requiring silicon dioxide to be melted in a crucible. As is known and appreciated by those skilled in the art, glass-forming materials such as silicon oxide, germanium oxide, etc. are materials that melt at high temperatures;
It is also an extremely good solvating agent for a wide variety of ions. Therefore, internal contamination of such materials is a serious problem, while the oxide precursor materials usually melt at lower temperatures and have lower solvation properties.

The principles described herein are for eliminating contamination of vitreous materials by producing them in an environment remote from the crucible.

As previously stated, the principles of the present invention may be advantageously used in the production of high-purity silica fibers, or the matrix material from which the fibers are made is easily layered and taupe. The present application is further advantageous for optical fiber manufacturing methods in that it can be alloyed, modified, or index-graded. As can be seen here, by providing an additional source of material in the process sequence, the silica fibers produced as described above can be made to have, for example, a refractive index gradient or a cladding layer on top of the own material. It can be further modified to include the following.

To change the refractive index of any of the multiple layers of fibers, an additional nozzle or other source of refractive index modifying agent, such as that shown in FIG. It can be used to provide refractive index modifiers towards

For example, a gaseous carbon source such as carbon tetrafluoride or a polyvalent metal source such as tin tetrachloride may be used. The additional reagent materials described above can be fed into the silicon stream from a single source mixed with oxygen gas, or alternatively can be fed simultaneously or sequentially with the oxygen from a separate source. . By controlling the concentration and composition of the refractive index modifying agent source, controlling the background pressure, and controlling the temperature of the forming fiber, the refractive index modifying component silicon and
• Diffusion into the silicon oxide material can be iteratively controlled to precisely define the refractive index gradient of the fiber.

The principles of the invention can also be used to provide cladding layers on fibers. As mentioned above, it is desirable for the cladding layer to have a slightly lower refractive index than the core layer to facilitate light retention within the core. In silica-based optical fiber systems, the core typically has a refractive index of 1.
466 and the cladding has a refractive index of 1.458.

Such a refractive index profile can be easily achieved in the present invention by including a small amount of halogen, such as chlorine or fluorine, in the 7-trix of the silicon oxide material. This inclusion, in accordance with the principles disclosed herein, releases a liquid stream of silicone, for example, and activates said liquid stream.
exposing the silicon oxide fibers to an atmosphere of activated halogen to produce silicon dioxide from the liquid stream; the activated halogens only partially diffuse into the silicon dioxide fibers; This can be easily achieved by not exposing it to conditions that are favorable for it. In this way, a cladding layer with a lower refractive index is formed on a core with a higher refractive index.

The cladding layer may be formed in a multi-station process as shown and described in FIG.

In some cases, the core fiber formed at the first station is fed to a subsequent station where an additional layer of a first component of crat, typically germanium or silicon, is applied to the core. After being exposed to an atmosphere containing activated oxygen and reactants such as halogens, said reactants are suitable for forming a cladding layer on the core. Multi-station coatings such as those described above may be used to form a protective layer around the core-clad composite to form a finished fiber optic fabric. The selection of preferably used protective coating materials is wide and includes ceramic coatings, vitreous coatings, and even organic polymeric coatings. The present invention can be used to deposit any of the coatings described above.

It is clear from the above description that the present invention is particularly suitable for the production of fiber optic nilemens I, since the method disclosed herein can be used for the production of multilayer structures, in particular concentric multilayer fibers. Coaxial optical fibers such as those described above can be manufactured from materials with very different optical properties, offering the installer of fiber optic elements the possibility of manufacturing unique devices. For example, a single fiber may include multiple concentric transparent layers separated from each other by cladding layers and opaque layers. Such a single fiber has the above structure,
Multiple separate data streams may be transmitted in parallel.

Although the application of the present invention to the production of fiber optic fiber optics has been described primarily with reference to materials based on germanium and silicon, this description has been made solely for ease of understanding. It should be pointed out that this is based on the fact that a limited range of materials such as those mentioned above are widely used commercially. However, the present invention may also be used to make optical fibers from materials that are not currently widely used because they may be difficult to form into fibers or may not be obtainable in pure form. It can be done. Such materials include semiconductor materials that have a band gap that provides high transparency in the infrared region of the spectrum. The semiconductor materials include chalcogen monomer materials, group (1) semiconductors, and group (2)-V semiconductors. Response properties, refractive index, thickness, etc. for fiber optical compositions may be obtained and better understood from U.S. Patent No. RE 28,028, republished June 4, 1974, and assigned to CorniBGlass Works Please note that.

(2) Production of iW Rim Ceramic 6 According to another embodiment of the present invention, a synthetically processed composite may be produced. The synthetic processing complex is shown schematically in Figures 9A and 9B. Figure 9A shows the powder material and Figure 9B shows the ribbon material.

The composite 101 has submicron to micron scale ceramic zones 105 and internal zones 103 of different compositions.
and a ceramic zone 105.

The ceramic zone 105, which is an island or layer and has a scale of less than 1 micron to about 0.0
It can have a thickness of 5 microns to about 20 microns. The maximum thickness is dependent on factors such as the kinetic, thermodynamic, and diffusion properties of the material used to form body 101, the microstructure of body 101, temperature, and reactants or oxidants.

The synthetically processed composite 101 is manufactured by first forming a body 101 that includes at least two different materials. The above materials are for single macroscopic use, realized for example by rapid solidification techniques. For example, melt spinning,
Any rapid solidification technique that results in a fine-grained microscopic structure may be used, such as sputtering, gas injection, melt jetting, CVD, plasma-assisted CVD, microwave-excited plasma-assisted CVD. The microscopic structure may be one or more of amorphous, microcrystalline, or polycrystalline, and may have crystalline inclusions.

The materials used to form body 101 include a pair of materials that differ significantly in their reactivity under the conditions used in ceramic formation. That is, in terms of reactivity, diffusivity, and/or morphology, the above two materials can realize the formation of a stable ceramic;
The other material then differs in such a way that it undergoes a chemical reaction at a slower rate or with a smaller penetration depth, or undergoes only a minimal chemical reaction.

Relatively active and relatively inactive materials differ in their rate of reaction with reactants, ie, oxidants.

For example, a relatively inactive metallic material will have a lower nitride formation kinetics than a relatively active material at the same temperature and nitrogen activity. Similarly, relatively inactive metallic materials have lower oxide formation reaction rates than relatively active materials at the same temperature and oxygen activity when the reactant is oxygen; has a lower carbide formation reaction rate at the same temperature and carbon activity, and has a lower boride formation reaction rate at the same temperature and boron activity if the reactant is boron.

Differences in reactivity are shown in Table 3 below by heat of formation of oxides and nitrides.

(T.B. Reed, “Free Energy of Binary Compound Formation: Chart Atlas for High Temperature Chemical Calculations (Free E
ner・gyof Formation of
Binary CompoundS: Al1
Eight Llasof Charts for Illight
Temperature Che+n1cal Ca
M, 1.T, r're
ss, Cambridge, Mass.

1971, ) 1 this 1 4L1 Fe -130,4 (1876') -
5,8(1809°)Co-114,2(17
68')Ni-114(1725')Ti
225 (1940°) -160,
5 (1940')V
-83,3 (2190°) Zr -
262 (2125°) , -163,8
(2128°)C[・-178,5(217
6°) -51(2176°)Mn
-192(2054°)Nb 192(
2218') -113,4(600')H
g −293 (1376° ) −
115,7 (1376°) No -107,
1 (1530') -31,9 (1150°)
Hf -265 (2495°) -88H-1
:113 (1748") Δl -467,8 (1743°)
-147,6 (2736°)Si -207
,1(169(io) -90(1680°
) Group III metals, ie iron, cobalt and nickel, as well as molybdenum and tungsten, have low negative heats of formation, indicating that these materials are considerably less reactive towards ceramic formation.

IVA group materials (Ti, Zr, Hf), V group materials (V
, Nb, Ta) and VI A group materials Fl (Cr, No
, W) and M8, A1 and Si have large negative heats of formation with respect to oxides and/or nitrides, indicating a rather high reactivity of these materials towards ceramic formation.

In terms of thermodynamic conditions, preferred reactive materials are Ti, Zr,
11f, ■, Nb, Ta, Cr, No, W, M
n, AI and Si, and C is a relatively non-reactive material that is preferred.

and Ni. However, kinetic and diffusion-related factors also have significance. Furthermore, because there are large differences in the heat of formation of oxides, nitrides, borides, or carbides within a group of reactive materials, for example (1) one or more of V, Cr, and Al as relatively unreactive materials; and (2) Zr, Ti as relatively reactive materials.
, Nb, Ilf, Mn, Ta, Cr, Hg, A1
and one or more of the above-mentioned materials ↑−
A pair may be configured. The difference in reactivity should be 4-minutes long enough to induce Cabrera-Mott diffusion. Preferably, the difference in the heat of oxide formation should be large enough to cause Cabler-Rahmot diffusion, leading to ceramic formation reactions.

In one embodiment, the relatively reactive materials include Ti, V, C
The metal material is selected from the group consisting of at least one of r, Zr, Nb, Hf, Ta, Al and Si, and the relatively non-reactive metal material is No, l'l, Fe.
, Co and Ni.

After formation of the microscopic body, the body is contacted with a highly excited reactant, ie, an oxidant.

The oxidant is a gaseous oxidant, and the reaction is a gas-solid reaction when the oxidant is nitrogen or oxygen. In the case of a pond, the oxidant can be carbon, boron, or a solid oxidant such as a reducible carbide, boride, nitride or oxide, where the reaction is a solid-solid reaction or a solid-liquid reaction. . Alternatively, the reaction may be a solid-liquid reaction or a liquid-liquid reaction. The excitation can be ion beam excitation, thermal excitation, electrical excitation, plasma excitation, microwave excitation, etc.

By contacting the body with the excited oxidant, the relatively reactive first material reacts with the oxidant, resulting in the formation of submicron to micron scale ceramic zones 105. Possibly as a result of Cabre-Lahmotte diffusion, a zone 103 is formed with an increased content of relatively unreactive materials. The above content increase is shown in Figures 10, 11A and 11B.

FIG. 10 shows a Ti-Zr-5i system in which the surface in contact with the nitrogen plasma is rich in titanium nitride and zirconium nitride, while containing no Si. That is,
Ti-t-Zr in titanium nitride-zircon nitride region
/Ti)-Zr + Si ratio is Ti + Zr/Ti in the starting material as well as in the non-nitrided region.
It is larger than the ratio of Ti + Zr + Si.

Figures 11A and 11B show Auger analysis of Ti-V-Al-Ni material before and after microwave plasma nitridation. The unnitrided specimen shown in Figure 11A exhibits a relatively constant metal concentration regardless of depth from the surface (left side of the graph). FIG. 11B shows a rapid increase in Ti and a decrease in Ni and other metals in the nitride region, and an increase in Ni in the non-nitrided region. That is, in the area that has not been nitrided, Ni
increases, and Ni decreases in the nitrided region.

The resulting synthetically processed complexes are flakes, chips, powders,
It can be in the form of a filament, wire or ribbon. This complex can be manufactured in various forms. for example,
By containing carbon, it can be formed into pellets. This means that carbon grains j′ are dispersed in the solid alloy, and the carbon base IT
This is achieved by forming the alloy into pellets I~ to obtain carbide-containing solid cermets I~.

In other cases, materials including filamentary and acicular materials as well as powdered materials may be formed into a pine I or body and adhered by a bonding agent such as molten metal or an organic polymer. Thus, according to yet another embodiment of the invention, a web of material that is substantially filamentary may be formed. The web is cooled or hardened in contact with a molten metal binder or an organic polymer binder to yield a bonded composite.

The method of the present invention can be modified in various ways without departing from the spirit and teachings of the main disclosure. Accordingly, the scope of the invention is limited only by the following claims.

[Brief explanation of drawings]

Figure 1 is a schematic cross-sectional view showing how the liquefied material flows out of the opening in the bottom of the crucible and is exposed to the excited diffusible modifying material; Figure 2 is the same as Figure 1; FIG. 3 is a schematic cross-sectional view showing when electromagnetic energy is used to generate eddy currents in a crucible and liquefied material stream that diffuse excited reforming material into a post 7 trix of liquefied material; FIG. A schematic cross-sectional view of the crucible and liquefied material stream of Figure 1 showing the case where two excited diffusible modifying materials come into contact with the liquefied material stream; Figure 4A is a schematic cross-sectional view of the crucible and liquefied material flow; 2 is a schematic diagram illustrating how the liquefied material flowing out of the liquefied material is deposited on the outer circumferential surface of the chill wheel after being modified by exposure to at least one excited modifier which preferably diffuses into the boss matrix of the liquefied material; FIG. 4B is a partially cross-sectional perspective view showing a first flow of liquefied material flowing out from an opening at the bottom of the crucible and a second flow of liquefied material pulled up from the bath by the outer peripheral surface of the wheel. A schematic, partially cross-sectional perspective view showing interaction with excited and introduced first and second species in the vicinity of the outer circumferential surface; FIG. 2 schematically shows a first deposition station containing a material stream and a plurality of deposition stations arranged in succession thereto containing a similar deposition structure suitable for the production of a multi-layered modified material; 6 is a top view of an irregularly shaped multilayer structure produced by deposition according to the principles of the present invention using a deposition apparatus such as that shown in FIG.
7D illustrate various excitation means for the gaseous components emanating from the nozzle shown in FIG. 3, ie microwave bone in FIG. 7A and 1- in FIG. 7B. f. Powered electrode, Figure 7C is induction heating coil, Figure 7D
Figure 8 is a schematic cross-sectional view showing a light-activated lamp; Figure 8 is a perspective view of an installation particularly suitable for mass production of synthetically processed materials, including the components of the deposition apparatus shown in Figures 1 to 7; , 9th A
9B and 9B are schematic isometric views of powder particles and ribbon portions nitrided according to a variation of the present invention, and FIG. 10 is a cross-sectional view of the synthesized composite ceramic material described in Example 1. Scanning electron micrographs of Figures 11A and 1IB are of the deposited fine-grained microstructure material of Example 2.
FIG. 2 is an explanatory diagram showing Auger analysis before and after nitriding treatment. 1... Deposition station, 3.23.33...
... Crucible, 1... Chamber, 5...
...Aperture, 6, 9.9a, 9b. 29, 39... Nozzle, 8a, 8b... Electrode, 8C... Induction coil, 17... Heating coil, 18... Hat, 21... ... Chill wheel, 60 ... Winding wheel, 62a,
62b...Microwave horn, 66...Heating Nilemene 1.68...Light source, 72...Reaction container, 73...
... Housing, 75 a - 75 d ... Pressure tank, 76 ... Temperature control coil, 77 ... Pressure conduit. Representative patent attorney Nakamura 1 ~ 5 Hθ7A FIG, 7B stomach -shi

Claims (134)

[Claims] (1) A method for producing a synthetically processed solid material, the method comprising the steps of supplying a first component and supplying a second component in a diffused form, the method comprising: applying an excited diffusible second component of the material to the first component; diffusing said second component into at least a portion of the first component; and determining the properties of each individual component. interacting a second component with the first component to form a synthetic solid material exhibiting a different range of properties. 2. The method of claim 1, wherein the first component is a flowing stream and the step of providing a flowing stream of the first component comprises providing a liquid flowing stream. 3. The method of claim 2, wherein the step of providing a liquid flow stream comprises the step of providing a stream of finely divided metal material. 4. The method of claim 2, wherein the step of providing a flow of liquid fluid comprises the step of providing a flow of micronized semiconductor material. 5. The method of claim 2, wherein the step of providing a stream of liquid fluid comprises the step of providing a stream of micronized ceramic material. (6) providing a flowing stream of the first component comprises providing a stream of material selected from the group consisting essentially of metallic materials, semiconductor materials, semi-metallic materials, ceramic materials, and combinations thereof; A method according to claim 2, characterized in that: (7) applying the excited diffusible second component to the flowing stream of the first component comprises guiding the excited gaseous material stream to impinge on the flowing stream of the first component; The method according to claim 2. (8) directing the flow of the excited gas material further comprises selecting the excited gas material from the group consisting essentially of nitrogen, oxygen, halogens, hydrocarbon gases, inert gases, hydrogen, vaporized alkali metals, and combinations thereof; 8. A method according to claim 7, characterized in that the method comprises: (9) applying the excited diffusible second component to the flowing stream of the first component comprises guiding the flowing stream of the first component through a plasma containing the second component; 9. The method according to claim 8, characterized in that: 10. The method of claim 8, further comprising the step of ionizing a second component of the synthetic material. 11. The method of claim 8, further comprising the step of radicalizing the second component of the synthetic material. 12. The method of claim 8, further comprising the step of thermally activating the second component of the synthetic material. (13) The method of claim 8, further comprising the step of exciting the second component by a photoactivation process. (14) The method of claim 8, further comprising the step of exciting the second component by a catalyst activation process. (15) The method of claim 1, further comprising the step of supplying the second component in a high pressure environment. (16) further directing the excited gas stream to impinge on the first component flow stream substantially in the direction of movement of the first component to transfer momentum to the first component flow stream; 8. A method according to claim 7, characterized in that the method comprises: 17. The method of claim 7, further comprising the step of maintaining contact between the flowing stream and the excited gas stream for a sufficient period of time to reach a desired degree of diffusivity. (18) The step of supplying a fluid stream of the first component of the material includes the steps of melting the first component in a crucible and injecting the first component as a fluid stream from the crucible. A method according to claim 2. 19. The method of claim 2, wherein the step of providing a flowing stream of the first component comprises injecting the first component through a pressurized nozzle. 20. The method of claim 2, wherein providing a flowing stream of a first component comprises overflowing the first component from the crucible. (21) supplying a flowing stream of the first component,
19. The method of claim 18, including the step of injecting the first component from an opening in the crucible. 22. The method of claim 21, further comprising the step of imparting a regular shape to the aperture. 23. The method of claim 21, further comprising the step of imparting an irregular shape to the aperture. (24) The method further comprises applying at least one energy burst to the first component to promote diffusion of the second component into at least a portion of the bulk of the host matrix of the first component. The method according to claim 2. (25) The method further comprises the step of utilizing electromagnetic energy to create eddy currents in the flow stream of the first component to promote the diffusion.
The method described in section. 26. The method of claim 24, further comprising the step of utilizing thermal energy to facilitate said diffusion. 27. The method of claim 2, further comprising the step of causing a third component of the excited diffusible material to act on the flowing stream of the first component. (28) The step of applying a third component to the fluid stream of the first component further comprises the step of supplying the third component as an excited fluid stream. the method of. (29) Furthermore, the excited diffusible second and third
28. The method of claim 27, comprising sequentially exposing a flowing stream of the first component to the components of the first component. (30) Furthermore, the excited diffusible second and third
28. The method of claim 27, comprising the step of simultaneously acting on the flowing stream of the first component. (31) The method according to claim 2, further comprising the step of guiding both components to a quenching surface after the interaction between the flowing stream of the first component and the second component has ended. Method. 32. The method of claim 31, wherein the step of guiding the first component and the second component to a quenching surface includes moving the quenching surface. (33) The method of claim 31, further comprising the step of controlling the temperature of the quenching surface. 34. The method of claim 2, wherein providing a fluid stream of the first component comprises directing the fluid stream to substantially surround the core member. . 35. The method of claim 9, further comprising the step of forming the plasma with AC energy. 36. The method of claim 9, further comprising the step of forming the plasma with microwave energy. 37. The method of claim 9, further comprising the step of forming the plasma with DC energy. (38) A method of making a relatively thick synthetically processed solid material comprising depositing first and second components of the solid material onto a core member, the method comprising: providing a core member; guiding the core member to at least one deposition station, each of the at least one station having the function of providing a flowing stream of a first component of material; a function of causing a second component to act on the fluid flow of the first component; and diffusing the second component into at least a portion of the fluid flow;
A method characterized in that the interaction of the second component and the first component each serves the function of depositing on the core a layer of synthetically processed solid material exhibiting a range of properties different from those of each individual component. 39. The method of claim 38, further comprising the step of providing a plurality of deposition stations and sequentially guiding the core to the plurality of deposition stations. (40) providing a flowing stream of a first component comprising providing a flowing stream of a first component formed from a material having a substantially similar composition to each of the plurality of deposition stations; 40. The method of claim 39, characterized in: (41) further comprising the step of forming a second component of material having a substantially similar composition in each of the plurality of deposition stations.
The method described in item 0. (42) The method further includes the step of forming, in at least one of the plurality of deposition stations, a second component of a material having a different composition from the material of the second component formed in the remaining deposition stations. 41. The method according to claim 40. (43) Furthermore, in at least one of the plurality of deposition stations, the first
40. The method of claim 39, including the step of forming a first component of material having a different composition than the materials of the components. 44. The method of claim 38, wherein providing a flowing stream of the first component comprises providing a liquid flowing stream. 45. The method of claim 38, wherein providing a flowing stream of the first component comprises providing a stream of finely divided metal material. 46. The method of claim 38, wherein providing a flowing stream comprises providing a stream of micronized semiconductor material. 47. The method of claim 38, wherein the step of providing a fluid stream comprises providing a flow of micronized ceramic material. (48) providing a flowing stream of the first component comprises providing a stream of material selected from the group consisting essentially of metallic materials, semiconductor materials, metalloid materials, ceramic materials, and combinations thereof; 39. The method of claim 38. (49) The step of causing the excited diffusible second component to act on the flowing stream of the first component comprises the step of guiding the excited gaseous material stream to impinge on the flowing stream of the first component. 39. The method of claim 38. (50) directing the flow of excited gaseous material further comprises selecting an excited gaseous material from the group consisting essentially of nitrogen, oxygen, halogens, hydrocarbon gases, inert gases, hydrogen, vaporized alkali metals, and combinations thereof; 50. The method of claim 49, comprising: (51) applying the excited diffusible second component to the flowing stream of the first component comprises guiding the flowing stream of the first component through a plasma containing the second component; 51. A method according to claim 50, characterized in that: 52. The method of claim 51, further comprising the step of ionizing a second component of the synthetic material. (53) The method of claim 51, further comprising the step of radicalizing the second component of the synthetic material. 54. The method of claim 51, further comprising the step of thermally activating the second component of the synthetic material. (55) The method of claim 51, further comprising the step of exciting the second component by a photoactivation process. 56. The method of claim 51, further comprising the step of exciting the second component by a catalyst activation process. (57) The method of claim 38, further comprising the step of supplying the second component in a high pressure environment. 58. The method of claim 57, further comprising configuring the core member to function as a mold for sequentially depositing layers of synthetically processed solid material. (59) The method further comprises the step of guiding the excited gas stream to impinge on the first component flow stream to transfer momentum to the first component flow stream. The method according to scope item 49. (60) The method further comprises maintaining contact between the flowing stream and the excited gas stream for a sufficient period of time to reach a desired degree of diffusivity of the second component in the host matrix of the first component. A method according to claim 49. (61) a first
Claim 38, wherein the step of providing a fluid stream of a component includes the steps of melting the first component in a crucible and injecting the first component as a fluid stream from the crucible. The method described in. (62) a first
39. The method of claim 38, wherein providing a flowing stream of a component includes injecting the first component through a pressurized nozzle. (63) a first
39. The method of claim 38, wherein providing a flowing stream of a component includes overflowing the first component from the crucible. (64) a first
39. The method of claim 38, wherein providing a flowing stream of a component includes injecting the first component from an opening in the crucible. 65. The method of claim 64, further comprising the step of imparting a regular shape to the aperture. (66) further comprising imparting an irregular shape to the aperture, interacting the second component and the first component to form a synthetically processed solid material having a corresponding cross-sectional shape; Claim 64, characterized in that the material is configured to function as a mold for sequentially depositing layers of synthetic processing material in a continuous deposition station to produce a final product of predetermined cross-sectional shape. The method described in. (67) Further, the first component at least one of the deposition stations is configured to facilitate diffusion of the second component in at least a portion of the host matrix of the first component.
39. The method of claim 38, comprising the step of subjecting the flowing stream of components to at least one energy burst. 68. The method of claim 67, further comprising the step of utilizing electromagnetic energy to induce eddy currents in the first component flow stream. 69. The method of claim 68, further comprising utilizing thermal energy to facilitate said diffusion. 38. The method of claim 38, further comprising the step of causing a third component of the excited diffusible material to interact with the flowing stream of the first component at at least one of the deposition stations. Method described. (71) The step of applying a third component to the fluid stream of the first component further comprises the step of supplying the third component as an excited fluid stream. the method of. (72) Furthermore, the excited diffusible second and third
71. The method of claim 70, comprising sequentially exposing a flowing stream of the first component to the components of the first component. (73) Furthermore, the excited diffusible second and third
71. The method of claim 70, comprising the step of simultaneously acting on the flowing stream of the first component. 38. (74) further comprising directing a flowing stream of the first component modified by the second component in at least one of the deposition stations to a quenching surface. The method described in. 75. The method of claim 74, wherein the step of guiding the first component and the second component to a quenching surface includes moving the quenching surface at high speed. 76. The method of claim 74, further comprising the step of providing temperature control of the quenching surface. (77) Claim 57 further comprising the step of forming the plasma using AC energy.
The method described in section. 78. The method of claim 57, further comprising forming the plasma with microwave energy. (79) Claim 57, further comprising the step of forming the plasma using DC energy.
The method described in section. 80. Claim 38 further comprising the steps of forming the relatively thick synthetically treated solid material as elongated fibers and collecting the fibers on a take-up spool. Method described. (81) further comprising configuring the take-up spool to provide a biasing force along a longitudinal direction of travel of the fibers, the force facilitating passage of the fibers through a plurality of deposition stations; 81. The method of claim 80, characterized in that: (82) A method for producing a light transmission fiber comprising reacting a first component stream and a second component to form a fiber, the method comprising: a first component stream selected from one or more Group IV elements; applying excited oxygen to the flowing stream; dispersing the excited oxygen into at least a portion of the flowing stream; and interacting the excited oxygen with the first component to form a synthetically processed optical transmission fiber. and a step of acting. 83. The method of claim 82, wherein the step of providing a fluid stream comprises providing a silicon fluid stream. (84) Claim 8, characterized in that the step of supplying a flowing stream supplies a flowing stream of germanium.
The method described in Section 2. 85. The method of claim 82, wherein providing a flowing stream comprises providing a flowing stream of silicon-germanium compound. 86. The method of claim 82, wherein the step of providing a flowing stream further comprises adding an additional polyvalent metal to the flowing stream. (87) The method further comprises the step of applying an excited third component containing one or more elements selected from the group consisting essentially of halogens, polyvalent metals, nitrogen, and alkali metals to the flowing stream. 83. The method of claim 82. (88) A method for producing a synthetically processed solid material by reacting a first component and a second component at a moving surface, the method comprising: contacting a first component, contacting a portion of the moving surface with a flowable second component of the material, substantially (
Catalytically introducing a third component of the excited material that is capable of diffusing into a component selected from the group consisting of: 1) the first component, (2) the second component, and (3) the first and second components. and diffusing a third component into at least a portion of the selected component, and causing the third component to catalytically interact with the selected component to form a synthetically processed solid material exhibiting a range of properties distinct from those of each said component. A method comprising the steps of: (89) The method of claim 88, wherein the step of deploying a moving surface further comprises the step of deploying a rotationally moving surface. (90) contacting at least a portion of the moving surface with the flowable first component further comprises liquefying the first component within the crucible; and ejecting the first component from the crucible as a flowing stream. 89. The method of claim 88. (91) The step of contacting at least a portion of the moving surface with the flowable first component further comprises the step of providing the flowable first component to the immersion bath. Method. (92) Contacting the first component portion of the moving surface with the flowable second component further includes melting the second component within the crucible and injecting the second component from the crucible as a flowing stream. 89. A method according to claim 88, characterized in that: (93) Claim 88, wherein the step of contacting the first component portion of the moving surface with the flowable second component further comprises the step of providing the flowable second component to the immersion bath. Method described. (94) The step of contacting at least a portion of the moving surface with the flowable first component further comprises the step of providing the flowable first component to the spray bath. Method. (95) Claim 88, wherein the step of contacting the first component portion of the moving surface with the flowable second component further comprises the step of providing the flowable second component to the spray bath. Method described. (96) The method of claim 88, wherein the step of catalytically introducing the excited third component further comprises the step of selecting the first component. (97) The method of claim 88, wherein the step of catalytically introducing an excited third component further comprises the step of selecting a second component. (98) The method of claim 88, wherein the step of catalytically introducing the excited third component further comprises the step of selecting the first and second components. (99) The method of claim 88, wherein the step of deploying a moving surface further comprises the step of deploying an excited diffusible moving surface. (100) Further, substantially (1) the first component, (2) the second component
(3) a third component, and (4) combinations thereof; diffusing the fourth component and catalytically interacting the fourth component with the selected components to form a synthetically processed solid material exhibiting a range of properties distinct from those of each individual component. 89. The method of claim 88. (101) further comprising providing a plurality of moving surfaces, wherein a portion of the surface of at least one of the plurality of moving surfaces substantially comprises (1) a first component; (2) a second component;
89. The method of claim 88, further comprising contacting a component selected from the group consisting of: (3) a third component; and (4) combinations thereof. 102. The method of claim 88, further comprising utilizing a magnetic energy field to create eddy currents in the flow stream of the first component to promote the diffusion. Method. 103. Claim 88, wherein the second component is ionized and the method further comprises utilizing an electromagnetic field to promote diffusion of the ions in the first material. The method described in. (104) Claim 2 further comprising the step of causing an unexcited component of the material to act on the flowing stream.
The method described in section. (105) A method of forming a synthetically processed composite material having sequentially a submicron to micron scale ceramic zone, an internal zone of different composition, and a ceramic zone, the method comprising: (a) a comparative 2 different materials comprising a relatively reactive first material and a relatively non-reactive second material.
(b) contacting the body with a highly excited reactant;
reacting a relatively reactive first material with a reactant to form a submicron to micron scale ceramic zone while maintaining an internal zone enriched with relatively non-reactive material; A method characterized by: (106) Claim 10, wherein the composition of the plurality of zones is a function of depth from the surface of the body.
The method described in Section 5. (107) The method according to claim 105, wherein the zone is an island. (108) A method according to claim 105, characterized in that the zone is a layer. (109) The method of claim 105, wherein the body further comprises a component that increases porosity. 110. The method of claim 105, characterized in that the highly excited oxidant is excited by a method selected from the group consisting of ion beam excitation, thermal excitation, and electrical excitation. (111) The method according to claim 6, characterized in that the highly excited oxidant is excited by microwave radiation. (112) the synthetically processed composite material is a synthetically processed cermet-type material comprising submicron to micron scale ceramic zones and metallic zones; (a) a relatively reactive first material; (b) contacting the body with a highly excited oxidizing agent;
reacting a relatively reactive first material with an oxidizing agent to form a submicron to micron scale ceramic zone while maintaining an interior zone enriched with relatively unreactive metallic material; 106. The method of claim 105. (113) At the same temperature and nitrogen activity, a relatively unreactive metallic material has a lower nitride formation reaction rate than a relatively reactive material.
The method described in Section 2. (114) At the same temperature and oxygen activity, a relatively unreactive metallic material has a lower oxide formation reaction rate than a relatively reactive material.
The method described in Section 2. (115) At the same temperature and carbon activity, a relatively unreactive metallic material has a lower carbide formation reaction rate than a relatively reactive material.
The method described in Section 2. (116) Relatively reactive materials include Mg, Ti, V, C
r, Zr, Y, Nb, Hf, Ta, Al and Si, and the relatively non-reactive metallic material is selected from the group consisting of Ho, W, Fe, Co and Ni. 113. The method of claim 112, wherein: (117) Relatively reactive materials include Ti, V, Zr, H
a relatively non-reactive first metal selected from the group consisting of at least one of Fe and Nb;
, Co, and Ni, the oxidizing agent is nitrogen, and the method comprises: (a) a relatively reactive first metal and a relatively unreactive second metal;
(b) contacting the body with microwave-excited nitrogen to transfer the relatively reactive first metal to the surface of the body and react with the nitrogen to form a 1-20 micron thick nitride layer; 117. The method of claim 116, wherein the method comprises forming a relatively unreactive metal-enriched underlayer while maintaining a relatively unreactive metal-enriched underlayer. (118) The method of claim 112, comprising forming a body having a fine-grained microstructure comprising a relatively reactive first metal and a relatively unreactive second metal. . (119) The method of claim 14, wherein the body has a fine-grained microstructure selected from the group consisting of at least one of amorphous, microcrystalline, and polycrystalline. (120) The method according to claim 118, characterized in that a fine-grained microscopic structure is formed by rapid solidification. (121) Claim 120, characterized in that the fine-grained microstructure is formed by a rapid solidification method selected from the group consisting of atomization, melt spinning, sputtering, CVD, plasma CVD, and microwave-excited plasma CVD. The method described in section. (122) The method according to claim 121, characterized in that a fine-grained microscopic structure is formed by melt spinning. (123) To form a layered nitride cermet-type synthetically processed composite material with a submicron-scale outer nitride layer and an inner metal layer: (a) at least one of Ti, V, Zr, Hf, and Nb; forming a molten alloy comprising a relatively reactive first metal selected from the group consisting of; and a relatively unreactive second metal selected from the group consisting of at least one of Fe, Co and Ni; (b) rapidly solidifying the alloy to form a solid alloy body with a fine-grained microstructure selected from the group consisting of amorphous, microcrystalline and polycrystalline; (c) subjecting the body to microwave-excited nitrogen; The relatively reactive first metal is transferred to the surface of the body and reacted with nitrogen to form a 1 to 20μ
113. The method of claim 112, comprising forming a thick nitride layer while maintaining an underlying layer of relatively unreactive metal from which relatively reactive metal has been removed. 124. The method of claim 123, comprising adding dispersed particulate carbon to the solid alloy and pelletizing the carbon-containing alloy to form a solid carbide-nitride cermet. (125) To form a layered oxide cermet-type synthetically processed composite material with a submicron-scale outer oxide layer and an inner metal layer, consisting of (a) at least one of Ti, V, Zr, and Nb; a relatively reactive first metal selected from the group;
(b) rapidly solidifying the alloy to form an amorphous, microcrystalline and a relatively non-reactive second metal selected from the group consisting of at least one of Fe, Co and Ni; (c) contacting the body with microwave-excited oxygen to transfer a relatively reactive first metal to the surface of the body; 1 to 20μ by reacting with oxygen
113. The method of claim 112, comprising forming a thick oxide layer while maintaining an underlying layer of relatively unreactive metal from which relatively reactive metal has been removed. (126) Claim 105, characterized in that two or more different materials including a relatively reactive first material and a relatively non-reactive second material include micron-scale flakes. Method described. (127) (a) First, contacting the body with a highly excited reactant causes the relatively reactive first material to react with the reactant to form a micron-scale ceramic zone while at the same time being relatively non-active. 127. The method of claim 126, comprising: maintaining a zone of concentrated reactive material; and (b) then bonding the micron scale flakes. (128) Claim 1 characterized in that micron scale flakes are bonded by plasma sintering.
The method described in Section 27. (129) Claim 105, wherein the two or more different bodies comprising a relatively reactive first material and a relatively non-reactive second material include substantially filamentary materials. The method described in section. 130. The method of claim 129, comprising: (a) forming a web of substantially filamentary material; and (b) combining the web with a binder to form a bonded body. . (131) The method according to claim 130, wherein the binder is a molten metal. (132) (a) forming a substantially filamentary material web comprising two or more different materials, including a relatively reactive first material and a relatively non-reactive second material; (b) Contacting the filamentary material with a highly excited oxidizing agent causes the relatively reactive first material to react with the oxidizing agent to form submicron-scale ceramic zones while leaving other zones relatively unreactive. (c) forming a web of filamentary material; (d) contacting the web with a molten metal binder; and (e) cooling the web to form a bonded composite material. 132. The method of claim 131, comprising the step of: (133) The method according to claim 132, wherein the binder is an organic polymer. 134. The method of claim 105, wherein the body comprising two or more different materials, including a relatively reactive material and a relatively non-reactive material, is a powder.