TWI307680B - Method for peoducing fe3o4-based magnetic nanowires - Google Patents

Description

130^8^396 3⁄4 Nine Patent Application Replacing Page (Amended in September, 1997) Description of the Invention: [Technical Field] The present invention relates to a method for manufacturing nanowires, It refers to a method for producing a magnetic nanowire body mainly composed of triiron tetroxide (Fe304). [Prior Art] The most common method for producing nanomaterials is the solution strategy reaction and vapor-solid reaction > wherein the naphthalene synthesized by gas-solid reaction method Rice materials generally have better crystalinity. However, for the synthesis of Fe304 nanowires, due to the influence of its cubic crystal structure and its intrinsic magnetism, it is impossible to automatically deposit atoms into a one-dimensional nanostructure via a gas-solid reaction pathway. At present, the synthesis of Fe304 nanowires is a hydrothermal method. For example, there is a hydrothermal method in which a surfactant is used in combination to dissolve a surfactant and a reactant to form a homogeneous aqueous solution (that is, an aqueous solution containing Fe3+ and Fe2+), and the homogeneous aqueous solution is placed. In an autoclave, while maintaining a working temperature between 100 ° C ~ 200 ° C for several hours, after several times of cleaning and vacuum drying to obtain Fe304 nanowire body, where The role of the surfactant is to limit the one-dimensional anisotropy growth of the Fe3〇4 nanowire. It is difficult to obtain a clean Fe304 nanowire because the surfactant is not easily removed after the reaction is completed. body. There is also a surfactant-free 1307680 method, which uses Fe3〇4 nanoparticles dispersed in an aqueous solution of sodium hydroxide (Na〇H) as a precursor (precurs〇r And placing the aqueous solution of sodium hydroxide dispersed in the card particles in U (rc~16〇. The pressure of the crucible is about 24 hours). The precipitate is filtered (precipkati〇n), washed, and vacuum dried. In addition, some people use the hydrothermal method of bow-in magnetic field to synthesize FhO4 nanowires. This method is to improve the sequelae caused by surfactants. Under the requirements of high-density recording and signal-to-noise rati〇, a single information bit (information bit) corresponding to a single material particle is used as a perpendicular recording media. The evolution direction of the future development of magnetic recording. Since the magnetic nanowire body and the nano cylinder (nan〇r〇ds) have a very small cross-sectional area and excellent aspect rati〇, they are used for vertical recording media. the best of Especially, Fe3〇4 nanowire, because it is one of the earliest magnetic materials used by humans, and it is also an oxide (making it have higher stability than general metal magnetic materials), so It has great potential in the future nano-scale magnetic recording applications. In addition, based on the intrinsic half-meta丨 characteristics of Fhh nanowires, it is also suitable for application; nanometers; (nan〇_Spintr〇njC to improve the electron spin selectivity (spin_selectivity). For the characteristics and applications of the above nano magnetic materials, it is even more possible to form an oxide layer on the surface of the Fe3〇4 nanowire body ( (10) ia iayer) to form a core-shell structure of Fe3〇4 nanowires. The speciar effect provided by the aforementioned oxide layer on the Fe3〇4 nanowire causes the electron 1307680 to The material interface produces specular reflection to reduce the irregular dispersion of electrons, thereby extracting the spin selectivity of the electrons and improving the efficiency of the nano-spintronic components. In the current technology, it is not easy to synthesize the core. It is Fe3〇4 and covers the one-dimensional structure of the nano-scale oxidation shell. In terms of common sense, if a 3〇4 nanowire body with an oxide shell structure is to be prepared, the steam-mine-ah (four) method is used. The use of an oxidizing atmosphere should be a reasonable choice, so the method can easily obtain the nano-shell of W. Although the steam-bonding method can coat the oxide layer on the surface of the MW nanowire, but in the process environment of the steam oxide oxide 'Easy to cause Fe3〇4 nanometer (4) to be oxidized to form ferric oxide (Fe2〇3) nanowires'. Therefore, the method of making the core-shell structure of Fe3〇4 nanowires by Xiangluo bond still has material oxidation. The problem exists. Too, from the above, it is known that a ferroferric oxide body having low impurities and excellent quality is prepared, and the problem of the formation of the outer shell layer is improved by reducing the structure of the ferro-nitride nanowire body and improving the core-shell structure. The ferroferric oxide nanowire is used by the technology to make the technology of the core structure of the ferroferric oxide nanowires. It is currently researched in the field of magnetoferric trioxide-based magnetic field. The goal to be worked hard. SUMMARY OF THE INVENTION <Summary of the Invention> Based on the prior art, the method for producing a % 〇 4 Nai liquid phase and the Hui Gutian gong is limited to an effective side: the problem that the agent is to be removed; and there is no specific effective method In order to produce a core-shell for use in a reducing environment, (iv) the present invention has the property of 3〇4, and (9)F-nf 2〇3) itself is easily reduced to an I-to-304 nanowire body. In addition, in combination with the cation source (cadon S〇Urce) which provides the oxide of the Fe3〇4 nanowire body in the reaction environment of the 7 1307680, the ho* nano-nuclear structure with the core-shell structure is firstly obtained. 'The present invention uses a plurality of 奈3 nanowires as a starting material for forming a % 〇 4 nanowire body (starting (8), and heating and providing the same to the Fe 2 〇 3 nanowire body - (4) uctive

Gaya Sphere) causes the a_Fe2〇3 nanowire to be reduced back to the nanowire body. In addition, the oxygen released by the a-Fe2〇3 nanowire body during the reduction of the 4 nanowire body is used as the oxygen ion source for forming the shell oxide; Heating of the solid cation source causes it to liberate M gas particles as a source of cations for forming the oxide.

It is worth mentioning that 'Phase transformatic mA Fe3〇4 nanowire body can be completed for the pure 2〇3 nanowire body, therefore, the temperature and heating of the a-Fe2〇3 nanowire body are implemented. The time must be at least 1 and minutes higher than the material. In addition, due to the higher temperature of the nano-wire body, the thermodynamic instability and kinetic factors of the material will cause the nanowire body to collapse. Or the a_Fe203 nanowires in contact with each other are free from damage due to the higher diffusion coefficient (Diffusivity). The final temperature of Fe3〇4 is 2〇3 nanowires. The temperature is up to 6〇 (rc. Therefore, in order to avoid the nanowire body, it is suitable to be implemented in the above a_. From the foregoing description, when the a_Fe2〇3 nanowire body is reduced back to the senna nanowire body, the oxygen released from the nanowire body can be In the presence of impurity atoms, the μ gas particles released from the U β 3 Μ and solid cation source react with each other and form directly on the surface of the _4 nanowire body—containing μ 1307680 with excellent quality and no oxidation problem. The oxide layer, which in turn produces Fe3〇4 with less impurities and core-shell structure The present invention is directed to a method for producing a magnetic nanowire body having a main body of tetraoxide. The other object of the present invention is to provide a The magnetic nano-wire body of tetraoxide. The main character of the horse is: Inventing a magnetic nano-based method based on triiron tetroxide, including the following steps (4) providing a plurality of first heating zones in the reaction chamber Iron nanowire body; - oxidation (b) decompression of the reaction chamber; (c) heating the reaction chamber; (4): introducing a reducing atmosphere into the reaction chamber; and (smelling the original atmosphere and the reaction The temperature of the chamber restores the α phase trioxo: the iron nanowire body to form a plurality of ferroferric oxide nanowires. 'The present invention is a magnetic nanowire body made by the aforementioned method. Emulsification-iron is the effect of the invention: it oxidizes the triiron nitrite and degrades: the oxidation problem in the case of a quadrupole-layer structure with low quality and excellent quality, and the manufacturing taste of the outer iron nanowire body, , the core of the structure of the four rolling three /, in order to make the core shell structure of the four oxygen The ferritic nanowire body is widely used by the technology industry. &Iron-Iron [Embodiment] 9 1307680 <Detailed Description of the Invention> The method for producing a magnetic nanowire body mainly composed of triiron tetroxide 'Includes the following steps: ' (4) in a reaction chamber - the first heating zone provides a plurality of nanowires of ferric oxide; (b) the reaction chamber is depleted; 0) the reaction chamber is added (d) introducing a reducing atmosphere into the reaction chamber; and (4) reducing the phase of the ferric oxide nanowire by the reducing atmosphere and the temperature of the reaction chamber to form a plurality of triiron telecommunications Line body. Preferably, after the step (4), the method further comprises a step (〇, the step () is to provide a M-containing and solid-state cation source in a second heating zone to which the β-anthracene reaction is caused, so that each α phase three When the ferric oxide nanowire body is reduced to a ferroitride tetraoxide body body, 'by forming a niobium-containing oxide layer on one surface of each of the ferroferric oxide nanowires to form a core-shell structure The ferrocene oxide _ $ linear body, and the reducing atmosphere of the step (4) is composed of a reducing gas and an inert gas. The hydrazine suitable for the step (a,) of the present invention is at room temperature. An element which is a solid phase oxide after oxidation; and the reducing gas suitable for use in the present invention is selected from the group consisting of hydrogen (Η,), carbon monoxide (C〇), ammonia (ΝΗ3), and alkane ( Alkane); more preferably, cerium is selected from the group consisting of cerium (Si), germanium (Ge), and a combination thereof. Preferably, the reducing gas is hydrogen and the inert gas is argon. Gas (Ar); the reaction temperature of the first heating zone is between 45 (rc~6〇〇.〇; this step 10 1307680 (e) The reaction time is at least greater than ίο minutes. More preferably, the reaction time 疋 of the step (e) is between 1Q minutes and 12G minutes; and the volume percentage of hydrogen in the reducing atmosphere is at least greater than 1 vol. More preferably, the volume percentage of hydrogen in the reducing atmosphere is between 1 vol% and 20 vol%. More preferably, the volume percentage of hydrogen in the reducing atmosphere is between 1 vol% and 10 vol. Between %. In a specific embodiment, the enthalpy of the step (a,) is 矽, and the volume percentage of hydrogen in the reducing atmosphere is between 2 vol% and 7 vol%; i also 5 rewards a 4 cylinder - the reaction temperature of the heating zone is between 80 (TC ~ 2000 ° C also ° Hai first heating zone reaction temperature is between 900 ° C ~ 1500. 〇 between ° The working pressure of the step (b) is between 〇] T〇rr~1〇〇T〇rr〇 在@在其他- specific embodiment, the step (&,) is wrong, hydrogen is in the The volume percentage in the original atmosphere is between 2 ν 〇 1% and 7 v 〇 1%; and the reaction temperature in the second heating zone of the 乂 乂 佳 地 is 7 〇〇. ~15〇(r 之 乜 rc rc rc 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 戎 rc rc rc rc rc rc rc rc rc In addition, the present invention can be made into a magnetic nanowire body mainly composed of triiron tetroxide by the above-mentioned method. The other technical contents, characteristics and effects of Guan Ben ^ Ming are described in the 'S 4 test pattern. In the detailed description of the six specific embodiments, it will be clearly shown. C Use material source > (8) 1307680 1. Wrong (Ge) block · Taken from silicon development international cooperation (SDIC) materials company Made and modeled. 2. Argon (Ar): Argon gas produced by Lianhua Gas Company with a purity greater than 99.995%. 3. Hydrogen (3⁄4): Hydrogen produced by Lianhua Gas Company with a purity greater than 99.995%.

<Specific Example> In one embodiment of the method for producing a magnetic nanowire body mainly composed of ferric oxide, this reduction atmosphere is composed of 2.5 ga and 47.5 sccm of Ar. The composition (ie, Η ν 〇 % % 斛 = 〇 = = = = = = = = = 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 The first heating zone in the reaction chamber provides a plurality of single crystal structures formed by a gas-solid reaction and has an average diameter of about several tens of nanometers.

The recording block of a technology G-1066' and the reducing atmosphere of the specific embodiment introduced into the reaction chamber causes the reaction environment of the reaction chamber to reach a force of (iv). In addition, a reaction temperature of 45 Gt is provided in the first heating zone and held for 2 G minutes to treat the a_

The Fe2〇3 nanowires are heated and cause the (6) nanowires to be reduced to Fe304 nanowires. Referring to Figure 1, the scanning electron microscope (scanning electron microscope (SEM) surface topography shows that the specific diameter of the a_Fe203 nanowire used in this embodiment of the present invention is about i 0. Between 5 〇 _. In addition, referring to Fig. 2 'shown by (4) surface topography, the (S) 12 1307680 specific embodiment - the nanowire body density obtained after the reduction reaction is reduced and the size is not significantly changed 'in addition, the surface exhibits a complex factor The a_F峨 nanowire body is a bump formed by damage during the reduction reaction. τ Referring to Fig. 3' is the transmission electron micr〇sc〇pe (hereinafter referred to as the transmission electron micr〇sc〇pe;

According to the figure, the shape of the nanowire is about 1 〇 nm in the shape of the top view (the upper left figure in Fig. 3); the selected area electron diffracti〇n, referred to as saed The graph shows (the upper right figure in Fig. 3) 'The crystal structure of the nanowire obtained from the z〇ne axis of [111] is %04 of the cubic phase; in addition, 'high resolution' The TEM (high resolution TEM; hereinafter referred to as HRTEM) image is not shown (the inset below in Fig. 3), and the nanowire of the first embodiment is grown along the [220] direction (i.e., [u〇] direction). And the interplanar spacing (d-spacing) of (4) and (2〇2) is 297.297 nm. &lt;Specific Embodiment 2&gt; The second embodiment of the present invention is a method for manufacturing a magnetic nanowire body mainly composed of triiron tetroxide. The second embodiment is substantially the same as the specific embodiment 1. The difference lies in the The reaction temperature of the first heating zone was 5 Torr. Hey. See Figure 4' for the SEM surface topography, due to 500. When the diffusion coefficient and the reaction rate of the ruthenium are greater than 450 ° C, the surface diffusion between the nanowires due to contact with each other causes some of the nanowires to melt together. Therefore, the surface of the specific embodiment after the reduction reaction Production increased. Referring to FIG. 5, the analysis data of the TEM of the specific embodiment 2 is shown by the TEM topography (the upper left diagram of FIG. 5), and the diameter of the 13 1307680 nanowire body of the specific embodiment 2 is about 10 nm; In addition, the SAED diagram shows (the upper right figure in Fig. 5) that the crystal structure of the nanowire obtained from the ribbon axis of [111] is the cubic crystal phase of Fe3〇4; in addition, it is shown by the HRTEM image (the illustration below in Fig. 5) The Fe3〇4 nanowire body of the second embodiment is grown along the [2 direction (ie, [Ϊ01] direction] and the surface spacing of the ceramics and (〇22) is 〇297. In the second embodiment, since the nanowire body phase changes to a nanowire body, it is produced in order to compensate for the lattice parameter (4) followed by (10)).

The distortion of the nanowire body during annealing ((10) jobs) is composed of a_Fe2〇3 and a crystal structure difference of 3〇4. &lt;Special Example 3&gt; The method of manufacturing a magnetic nanowire body mainly composed of ferric oxide is the same as that of the second embodiment, and the difference lies only in The average diameter of the a_Fe2〇3 nanowire body used in the specific three is about tens to two hundred nanometers. Referring to Fig. 6, the SEM surface topography shows that the average diameter of the ferritic oxide nanowire formed after the reduction in the third embodiment is about several tens to two hundred nanometers. The Fe304 nanowire prepared by the third embodiment of the present invention is dropped on the upper surface of one of the core substrates, and further the magnetic field is applied to the germanium substrate parallel to the main π t , π π % 4 The applied magnetic field on the upper surface of the substrate. Referring to Fig. 7', the SEM surface topography of the second embodiment of the present invention is q μ _ _. Because of this specificity, only one case of the two produced Fe304 contends @e & μ, + 4 does not have the small scale and appearance of the wood body itself with a high aspect ratio (four) (10) handsome. The characteristics of the nanowire body should be in the form of a single magnetic domain (four) gle d (10) ain). According to the observation of _, it can be found that the arrangement direction of the nanowire body tends to be parallel to the direction of the applied magnetic field 14 1307680. Referring to FIG. 8 and FIG. 9, respectively, the third embodiment of the present invention is a vibrating sample magnetometer ( Vibrating-sample magnet〇meter, abbreviated vsm) A hysteresis curve measured under analytical conditions in which the direction of the magnetic field is parallel and perpendicular to the upper surface of the substrate. When the direction of the magnetic field is parallel to the direction in which the nanowires are arranged, the magnetic field strength (ie, the H value) required to achieve the saturation magnetization value (ie, the enthalpy value) is low, and when the magnetic field direction is perpendicular to the arrangement direction of the nanowires. , it is not easy to achieve magnetic saturation. This phenomenon is due to the high aspect ratio of the Fe3〇4 nanowire itself, resulting in a highly anisotropic magnetic anisotropic, thus causing different reversal fields in different measurement directions. &lt;Detailed Embodiment 4&gt; The fourth embodiment of the present invention is a method for manufacturing a magnetic nanowire body mainly composed of triiron tetroxide. The fourth embodiment is substantially the same as the specific embodiment 1. The difference lies in the The reaction temperature in the first heating zone was 6 Torr. Hey. Referring to FIG. 10, the SEM surface topography shows that the atomic bonding and surface diffusion of the nanowires in contact with each other during the reduction show that most of the nanowires exhibit a branched state. The surface topography, and the specific yield of the Fe304 nanowire obtained after the reduction reaction is lower. Referring to Fig. 11 is an analysis data chart of the TEM of the fourth embodiment, which is shown by the TEM topography (the upper left diagram of Fig. 11), and the diameter of the nanowire body of the fourth embodiment is about 10 nm; The figure shows (the figure at the top right of Figure η), the crystal structure of the nanowire obtained from the ribbon axis of [110] is the cubic phase of FesO4; in addition, it is shown by the HRTEM image (inset below Figure 11) 15 1307680, The Fe3〇4 nanowire body of the fourth embodiment is grown along the mesh direction (i.e., [101] direction) and (the interplanar spacing of 2刼 is 〇24 nm. Referring to Fig. 12, the a-Fe2〇3 crystal The phase change is the evolution of the Fe3〇4 crystal/, and the direction perpendicular to the paper surface is the close packing of the atoms (the ci〇Sed sound (four) direction) (ie, the a-Fe2〇3 crystal and the Fe304 crystal are closely packed in the oxygen ion packing direction. It is [_ and [(1)]), and the solid arrow indicates the stacking direction of the anions (ie, oxygen ions) on the close packed surface.

According to the theoretical mechanism of the single-molecule reaction (unim〇lecular reason) of this phase change and the observation of the specific embodiment-four of the present invention, the a-Fe 0 crystallite can be adjusted by stacking order along the dense packing direction ( That is, the stacking order of the ababab... mode) is converted into a transistor crystal (ie, the stacking order of the ABCABC, the mode). And adjusting the stacking order (4), (4) will cause the atomic rearrangement of the close packed surface to cause the relative orientation of the close packed surface to rotate, and η because the Fe3〇4 crystal has a larger lattice constant (10)^c__), so that The process is more likely to happen. These reasons eventually lead to the reduction of the rice noodle body along the direction of the close packing of the oxygen material perpendicular to the Fe3G4 nanometer (4) (ie, the &lt;110&gt; direction family', eg [call, [call, [then], [(10)

, [〇li]) and &lt;111&gt; direction families become ♦. It is noted that the oxygen ion close packing direction of the above e3〇4 crystal of the present invention is exemplified by [111], and is suitable for: the oxygen ion close packing direction of the Fe3〇4 crystal of the present invention is The direction that satisfies the symmetry of the Japanese body structure (ie, the &lt;lu&gt; direction family). &lt;Specific Embodiment 5&gt; The present invention is a fifth embodiment of a method for producing a magnetic nanowire body mainly composed of arsenic pentoxide, and iron. The second embodiment is the same, and the difference of 1307680 is only that the second heating zone is provided with a germanium wafer (ie, in the fourth embodiment, the germanium is germanium), and the reaction temperature of the second heating zone is 1 〇〇〇°C.

Referring to FIG. 13, the analysis data of the TEM of the fifth embodiment is shown by TEM; the image of j is shown (the lower left side of FIG. 13), and the diameter of the nanowire of the fifth embodiment is about 40 nm~ Between 50 nm; another SAED diagram shows (pictured at the top left of Figure 13), the crystal structure of the nanowire obtained from the ribbon axis of [112] is the cubic phase of Fe3〇4; in addition, it is shown by the HRTEM image ( Fig. 13 is a diagram on the right side), the Fe3〇4 nanowire body of the fifth embodiment is grown along the [in] direction and the interplanar spacing of (〇22) and (2〇0) is 〇·3〇6, respectively. Nm and 0.428 nm, and the amorphous layer located on the periphery of Fe3〇4 is a cerium oxide (SiOx) layer containing cerium nanoparticles. Therefore, the ferrotitanium oxide prepared by the manufacturing method of the fifth embodiment is The main magnetic nanowire body is a Fe3〇4 nanometer body with a core-shell structure of a ruthenium oxide layer. In addition, referring to Figure 14, the TEM's high-angle annular dark field (five) clock annular angle dark fie丨d; referred to as HAADF) image and its energy dispersive spectrometer (abbreviated as "5") phantom composition analysis No, the periphery of the FesO4 nanowire body of the fifth embodiment is indeed a oxidized stone layer containing 6 rythr nanoparticles. &lt;Specific Embodiment 6&gt; The sixth embodiment of the present invention is a method for manufacturing a magnetic nanowire body mainly composed of triiron tetroxide. The sixth embodiment is substantially the same as the fifth embodiment, and the difference is only in the case of Μ Yes, and the reaction time is maintained for 9 minutes. See Figure 15 for the analysis data of the brain of the specific embodiment 6, 17 1307680 is shown by the TEM topography (the lower left in Fig. 15), the diameter of the nanowire of the specific embodiment is about 20 nm. Between ~30 nm; another SAED diagram shows (pictured at the top left of Figure 15) 'The crystal structure of the nanowire obtained from the crystal axis of [1 〇1] is the cubic phase of FesO4; in addition, it is shown by HRTEM image (Fig. 15 right illustration), the Fe3〇4 nanowire body of the sixth embodiment grows along the [2〇2] direction (i.e., [101] direction), and the interplanar spacing of (士) is 〇. 25 faces, and the amorphous layer located on the periphery of FesO4 is a layer of yttrium oxide (Ge〇x). Therefore, the magnetic nanowire mainly composed of triiron tetroxide prepared by the manufacturing method of the sixth embodiment The body is a Fe3〇4 nanowire body having a core-shell structure of a ruthenium oxide layer. Further, referring to Fig. 16, the analysis of the HAADF image of the TEM and its EDS shows that the periphery of the FhO4 nanowire of the sixth embodiment is a ruthenium oxide layer. It is worth mentioning that when the oxide layer is coated in the fifth embodiment and the sixth embodiment, the oxidation degree of the outer oxide layer can be changed by modifying the process parameters. Therefore, in the sixth embodiment The oxide layer is present without the wrong nanoparticle. The invention directly utilizes the a-Fe2〇3 crystal itself to directly reduce the reducing property of the Fe3〇4 crystal to obtain a FhO4 nanowire body. In addition, in combination with providing a source of cation (ie, M gas particles) during the reaction, the oxygen released from the nanowire body can be free of impurities when the a_Fe2〇3 nanowire body is reduced back to the FqO4 nanowire body. In the environment where the atom exists, it simultaneously reacts with the arriving M gas particles, and directly combines on the surface of the Fe3〇4 nanowire to form an oxide layer containing μ, thereby obtaining less impurities, excellent quality, and no FhO4 oxidation problem. Fe304 nanowire body with core-shell structure. 18 1307680 • The above-mentioned Xe method of the magnetic nanowire body mainly composed of triiron tetroxide according to the present invention can produce a ferritic trioxide IE Pf low in low impurity and excellent in quality. The oxidation problem of the ferric oxide nanowire body in the production of the outer cladding structure is such that the ferroferric oxide nanowire body having a core-shell structure is widely utilized by the technology industry, and the object of the present invention is indeed achieved. - The above is only the preferred embodiment of the present invention, and if not, 2X is limited to the scope of the present invention, that is, according to the patent 351® and the description of the invention in the present invention. Simple equivalent changes and modifications are still within the scope of the invention. BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1A is a top view of an SEM surface, illustrating a method for producing a magnetic neviline body mainly composed of triiron tetroxide according to the present invention, and a-Fe2〇 used in the first embodiment. 3 nanowire body; Fig. 2 SEM surface topography, illustrating the Fe3〇4 nanowire body prepared by the specific embodiment of the present invention after the reduction reaction; • Fig. 3 TEM analysis data diagram, illustrating The microscopic morphology and crystal structure of the specific embodiment of the invention; _ ^ 4 is - SEM surface topography, illustrating the invention - a specific embodiment - prepared after the reduction reaction] pe3 〇 4 nanowire body; ® 5 is a TEM analysis data diagram illustrating the micromorphology and crystal structure of the second embodiment of the present invention; • _ ® 6 is a SEM surface topography diagram illustrating the present invention - specific example 2 in the reduction reaction After the production! Figure 4 is a SEM surface topography diagram illustrating the specific embodiment of the present invention. 19 8 1^07680 2: 4 nanowire body is subjected to an external magnetic field. Figure 8 is a view of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The measured direction of the direction in which the line body is arranged is parallel to the nanograph 9. This is a specific embodiment of the present invention: a graph; the direction measured under the analysis condition of the line body is perpendicular to The nanograph 10 is—(10) the surface topography of Fig. 1 and the second graph; the fourth Fe3〇4 nanowire body obtained after the reduction reaction&quot;-specific embodiment FIG. 11 is a TEM analysis data diagram, TO ^ + invention § hai specific embodiment 4 of the microscopic morphology and crystal structure; F. Figure 12 is a crystal phase evolution diagram 'illustration, the crystal phase change is the crystal phase evolution of the e3〇4 day; FIG. 13 is a TEM analysis data diagram illustrating the microscopic morphology and crystal of a specific example 5 of the present invention. Figure 14 is a compositional analysis diagram of the Haadf image and its EDS of the specific example 5 of the present invention; Figure 15 is a TEM analysis data diagram illustrating the microscopic appearance of a sixth embodiment of the present invention. And a crystal structure; and Fig. 16 is a compositional analysis diagram of the HAADF image of the TEM of the sixth embodiment of the present invention and its EDS. 20 1307680 [Explanation of main component symbols]

21 8

Claims (1)

13076^94143396 invention patent application application ^ patent van g replacement page (97 car i face π:,, ten, the scope of application for patent: year f Μ曰 repair (2) positive replacement,: ._______ &quot; .... .I Wl If - L A method for producing a magnetic nanowire body mainly composed of triiron tetroxide, comprising the following steps (a) providing a plurality of 〇t phase three oxidations in a first heating zone in a reaction chamber Iron nanowire body; , (b) decompressing the reaction chamber; (c) heating the reaction chamber; (d) introducing a reducing atmosphere into the reaction chamber; (e) reducing the α phase ferric oxide ferric chloride body by the reducing atmosphere and the temperature of the reaction chamber to form a plurality of ferroferric oxide nanowires. 2. The method for manufacturing a magnetic nanowire body mainly composed of triiron tetroxide according to the patent application, further comprising a step (a) after the step (a), the step (a) ,) is provided in the second heating zone of the reaction chamber - a cation-containing and solid-state cation source, such that each α-phase ferric oxide nanowire is reduced to a triiron tetroxide body, thereby Forming a yttrium-containing oxide layer on one surface of each of the ferritic oxide nanowires to obtain a ferrocene oxide nanowire body having a core-shell structure, and the step (&amp;,) is in the chamber The enthalpy of the element _ oxide and the enthalpy of this step after oxidation is selected from the group consisting of hydrazine, hydrazine and a combination thereof. 3. According to the special shooting machine, please refer to the manufacturing method of the gangue wire which is mainly composed of triiron tetroxide in the second item. The Μ of this step (&amp;,) is 矽. 4. The method for producing a hetero-nanowire body mainly composed of triiron tetroxide according to claim 3, wherein the reaction temperature of the second heating zone is 800. (:~20〇〇.(: Between. 5. According to the patent, please refer to the patent application for the invention of the patent application No. 23 13 Ο 76 § 143396 _Please refer to the patent field replacement page (revised in September 1997). The reaction temperature of the second heating zone is between 90 (TC~1500 °C - 6. According to the second paragraph of the patent application scope The method for producing a magnetic nanowire body mainly composed of triiron tetroxide, wherein the enthalpy of the step (a,) is 锗. 7 -&gt; The method for manufacturing a rice noodle body, wherein the reaction temperature of the second heating zone is between 700 ° C and 1500 ° C. 8. The method for producing a magnetic nanowire body mainly composed of triiron tetroxide according to the seventh aspect of the patent application, wherein the reaction temperature of the second heating zone is between 9 〇〇〇 c and 12 (8). Between c. • According to the method for manufacturing a magnetic nanowire body mainly composed of triiron tetroxide as described in the patent application scope f1, the frequency of the (6) is composed of county gas and an erotic gas. The reducing gas is selected from the group consisting of chlorine gas, carbon monoxide, ammonia gas and alkane. 1 . According to the method for producing a heterogeneous nanowire body mainly composed of triiron tetroxide according to claim 9 of the patent application scope, the gas of the county is hydrogen gas, and the neon is ammonia gas. • A method of producing a tetragonal body of ferroferric oxide according to the cap patent I, K, wherein the volume percentage of hydrogen in the reducing atmosphere is at least greater than 1 V〇l%. • According to the method of (4) special ·M u, the method of making the rice noodles to avoid the nano line is the volume percentage of chlorine in the original atmosphere is 丄 v〇l ° /. ~20vol% between. The magnetic nano-wire gas mainly composed of triiron tetroxide is a manufacturing method in which the percentage of the replenishing SI towel is between 1 and 13 according to the patent application scope, wherein the hydrogen vol% Between ~10vol%. 24 13 Ο 7 6 143396 Inventive Patent Application Replacement Page (Amended in September 1997) 14_The magnetic nanowire body based on triiron tetroxide as described in Item 13 of the patent application scope The manufacturing method, wherein the volume percentage of hydrogen in the reducing atmosphere is between 2 vol% and 7 vol%. 15. The method for manufacturing a magnetic nanowire body mainly composed of triiron tetroxide according to claim 14 of the patent application, wherein the working pressure of the step (b) is between 0.1 Torr and 1 Torr. Between Torr. 16. The method according to claim 1, wherein the reaction temperature of the first heating zone is between 45 (TC and 600 ° C). 。. The method for producing a magnetic nanowire body mainly composed of triiron tetroxide according to the first aspect of the patent application 'wherein the reaction time of the step (e) is at least more than 10 minutes. A method for producing a magnetic nanowire body mainly composed of triiron tetroxide according to Item 7 of the patent application, wherein the reaction time of the step (e) is between 10 minutes and 120 minutes. 25