WO2006043407A1 - 非強磁性物質成形体の製造方法、及び非強磁性物質成形体 - Google Patents
非強磁性物質成形体の製造方法、及び非強磁性物質成形体 Download PDFInfo
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Definitions
- the present invention relates to a method for producing a non-ferromagnetic material molded body, and more specifically, a method for producing a non-ferromagnetic material molded body having anisotropy in magnetic susceptibility with controlled crystal orientation.
- the present invention relates to a molded ferromagnetic material.
- Ceramic materials widely used as materials for electronic components are known to have crystal axis orientation orientation that contributes to improving various characteristics of electronic components. Research and development related to you are actively underway. In particular, in the field of piezoelectric components, lead-based piezoelectric ceramic materials such as lead zinoleconate titanate (PZT) have been used, but lead-free piezoelectric ceramic materials that do not contain lead due to environmental considerations. If the piezoelectric properties such as the electromechanical coupling coefficient can be improved by controlling the orientation of the crystal axis, it is promising as an alternative to lead-based piezoelectric ceramic materials.
- PZT lead zinoleconate titanate
- a slurry is prepared by adding a solvent to a powder containing 90% by weight or more of a bismuth layered compound as a ceramic raw material powder, and a magnetic field of 1T (Tesla) or more is applied to the slurry in one direction.
- a method for producing a bismuth layered compound sintered body in which the slurry is solidified while the bismuth layered compound powder is oriented in a crystal plane perpendicular to the c-plane has been proposed (Patent Document). 1).
- Patent Document 1 focuses on the fact that a bismuth layered compound is a non-ferromagnetic material having anisotropy in magnetic susceptibility, and by applying a molding process to the slurry while applying a magnetic field in one direction. A crystal axis having a large magnetic susceptibility is oriented in the direction of the magnetic field, thereby making it possible to easily obtain a molded body without requiring a complicated manufacturing process.
- Patent Document 1 has a greater degree of freedom in the thickness of the molded body than the conventional so-called sheet method, and crystal orientation is performed for non-ferromagnetic materials having anisotropy in magnetic susceptibility. It can be applied to many substances.
- a ceramic slurry containing nonmagnetic ceramic particles is used.
- An unoriented sheet with a predetermined thickness is produced by coating on the base film, and the unoriented sheet is fed to the magnetic field application device while being supported on the base film, and a magnetic field in a predetermined direction is applied to the unoriented sheet.
- a non-magnetic ceramic particle is oriented in the direction of a magnetic field to produce an orientation-treated sheet, and the orientation of at least some of the non-magnetic ceramic particles in the orientation-treated sheet is fixed to obtain an orientation-fixed sheet.
- Patent Document 2 A method for manufacturing ceramic parts has been proposed (Patent Document 2).
- Patent Document 2 As shown in FIG. 7, an unoriented ceramic green sheet 101 is intermittently run in the direction of arrow a while being supported by a base film 102, and a first magnetic field application region 103 is obtained. Then, a magnetic field in a predetermined direction is applied to the ceramic green sheet 101, and ultraviolet rays are irradiated from above through the mask 104 in which the translucent portion 104a is provided in the vicinity of the end of the first magnetic field application region 103. After the matrix-shaped first orientation fixing part 105 is formed, a magnetic field is applied in the second magnetic field application region 106 in a direction different from the application direction of the first magnetic field application region 103, and then the second magnetic field is applied. A method is disclosed in which the second alignment fixing portion 108 is obtained by irradiating ultraviolet rays from above in the vicinity 107 of the application region 106 to fix the alignment of portions other than the alignment fixing portion 105.
- Non-ferromagnetic powder having a crystal structure other than equiaxed crystal is dispersed in a solvent, and the slurry is solidified and formed in a magnetic field and then sintered.
- Patent Document 3 A method for producing a ceramic sintered body has been proposed.
- Patent Document 3 discloses that the orientation can be controlled by solidifying a slurry in a magnetic field even for a non-ferromagnetic material such as an alumina ceramic sintered body.
- Patent Document 1 Japanese Patent Application Laid-Open No. 2002-121069
- Patent Document 2 Japanese Patent Application Laid-Open No. 2004-6704
- Patent Document 3 Japanese Patent Laid-Open No. 2002-193672
- Patent Document 1 Although the crystal axis orientation with the highest magnetic susceptibility can be oriented, other crystal axis orientations cannot be oriented.
- the a-axis can be obtained like a bismuth layered compound.
- b-axis susceptibility is almost equivalent
- c-axis susceptibility is a-axis and b-axis magnetization
- orientation cannot be imparted to the C-axis, so that it could not be used for applications requiring C-axis orientation.
- Patent Document 1 Although the a-axis or b-axis can be provided with orientation, the c-axis cannot be aligned in a certain direction in an arbitrary direction. From Table 1, we have been unable to use it for applications that require c-axis orientation.
- Patent Document 2 magnetic field application is performed twice on the ceramic green sheet 101 from different directions in the first and second magnetic field application regions 103 and 106.
- the first orientation fixing unit 105 is oriented in the vertical direction
- the second orientation fixing unit 108 is eg horizontal.
- the c-axis is smaller than the a-axis and b-axis, and the c-axis is not oriented in the direction of the magnetic field, and the c-axis is not intended to be oriented in a certain direction.
- Patent Document 3 discloses only one application of a force magnetic field that can select an arbitrary orientation direction by applying a magnetic field from an arbitrary direction. It is considered that the orientation of only a specific crystal axis selected by the force S is intended.
- the present invention has been made in view of such circumstances, and can provide orientation not only to a crystal axis having a maximum magnetic susceptibility to a magnetic field but also to other crystal axes. It is an object of the present invention to provide a method for producing a ferromagnetic material molded body and a non-ferromagnetic material molded body.
- the inventors of the present invention have intensively studied to achieve the above-described object.
- a magnetic field with a predetermined direction is applied to the ceramic slurry to impart orientation to the crystal axis with the maximum magnetic susceptibility, and the orientation is achieved.
- orientation can be imparted to crystal axes other than the crystal axis where the magnetic susceptibility to the magnetic field is substantially maximum. I got the knowledge that I can do it.
- the present invention has been made based on such knowledge, and the method for producing a non-ferromagnetic material molded body according to the present invention includes a slurry containing a non-ferromagnetic material having anisotropy in magnetic susceptibility.
- the "crystal axis having the maximum magnetic susceptibility with respect to the magnetic field” means, for example, that the magnetic susceptibility is lower than the crystal axis with the maximum true susceptibility, and that the susceptibility is not the maximum. However, in the behavior with respect to the magnetic field, it means a crystal axis that cannot be distinguished from the crystal axis with the maximum true magnetic susceptibility.
- the first orientation imparting step and the second orientation imparting step described above are continuously performed without any time interval.
- the orientation of the crystal axes other than the first crystal axis can be improved as compared with the case where the time interval is set.
- the method for producing a non-ferromagnetic material molded body of the present invention is characterized in that the first orientation imparting step and the second orientation imparting step are continuously performed.
- the method for producing a non-ferromagnetic material molded body of the present invention is characterized in that the viscosity power of the slurry produced in the slurry production step is 30 to 200 mPa's.
- the present invention can exhibit particularly remarkable effects in a bismuth layered compound having a large difference in magnetic susceptibility between the a-axis and b-axis of the crystal axis and the c-axis.
- the method for producing a non-ferromagnetic material molded body of the present invention is characterized in that the non-ferromagnetic material is a ceramic material mainly composed of a bismuth layered compound.
- the non-ferromagnetic material molded body of the present invention is a non-ferromagnetic material molded body obtained by subjecting a slurry containing a non-ferromagnetic material having anisotropy in magnetic susceptibility to a molding process while applying a magnetic field. It is characterized in that orientation is imparted to crystal axes other than the first crystal axis in which the magnetic susceptibility of the crystal axis with respect to the magnetic field is substantially maximum.
- the present invention can exhibit particularly remarkable effects in a bismuth layered compound having a large difference in magnetic susceptibility between the a-axis and b-axis of the crystal axis and the c-axis. Therefore, the non-ferromagnetic material molded body of the present invention is characterized in that the non-ferromagnetic material is a ceramic material mainly composed of a bismuth layered compound, and the crystal axis other than the first crystal axis is the c-axis. Yes.
- the orientation of crystal axes other than the first crystal axis can be further improved. It becomes possible.
- the viscosity power of the slurry prepared in the slurry preparation step is 30 to 200 mPa's, not only the crystal axis with which the magnetic susceptibility to the magnetic field is substantially maximized, but also the orientation of other crystal axes The property can also be improved.
- the non-ferromagnetic material is a cement containing a bismuth layered compound as a main component. Because it is a ceramic material, orientation can be imparted to the crystal axis, not only the a-axis and b-axis, which have substantially the same magnetic susceptibility, but also to the c-axis with the smallest crystal axis, and the piezoelectric ceramic material contains lead. Even if it is not, it is possible to realize various piezoelectric parts having excellent piezoelectric characteristics.
- the non-ferromagnetic substance molded body of the present invention is a non-ferromagnetic substance composition obtained by subjecting a slurry containing a non-ferromagnetic material having anisotropy in magnetic susceptibility to a molding process while applying a magnetic field. Even if it is a shape, not only the first crystal axis, which has substantially the highest magnetic susceptibility with respect to the magnetic field, but also the orientation is given to crystal axes other than the first crystal axis. Therefore, it can be used effectively in applications that require orientation in a crystal axis other than the first crystal axis.
- the non-ferromagnetic material is a ceramic material whose main component is a bismuth layered compound, and the magnetic susceptibility is approximately the same as the a-axis and b-axis. Orientation is given to the c-axis with the lowest magnetic susceptibility.
- a non-ferromagnetic material molded body having a high orientation of the c-axis, which is the longest axis among the crystal axes of the bismuth layered compound, can be obtained, and various piezoelectric parts having excellent piezoelectric characteristics when an electric field is applied can be obtained.
- FIG. 1 is a production process diagram showing one embodiment of a method for producing a non-ferromagnetic substance molded body according to the present invention.
- FIG. 2 is a perspective view schematically showing a superconducting magnet used in the above embodiment.
- FIG. 3 is a diagram showing an outline of a mud filling apparatus used in the embodiment.
- FIG. 4 is a perspective view of a ceramic sintered body produced in this example.
- FIG. 5 is a perspective view of a piezoelectric ceramic body obtained by cutting out the ceramic sintered body of FIG.
- FIG. 6 is a perspective view showing an appearance of a piezoelectric component obtained in an example.
- FIG. 7 is a plan view of a ceramic green sheet for explaining the method of manufacturing a piezoelectric ceramic component disclosed in Patent Document 2.
- FIG. 1 is a production process diagram showing a method for producing a non-ferromagnetic substance according to the present invention.
- a slurry containing a non-ferromagnetic material having anisotropy in magnetic susceptibility as a main component is produced.
- non-ferromagnetic materials having anisotropy in magnetic susceptibility include CaBi TiO, B
- Tungsten bronze type compounds such as SrNb ⁇ , BaNb ⁇ , Ho Ti ⁇ , Dy Ti
- Pycroa compounds such as 7 and ceramic materials such as ZnO are practical for use in electronic parts, and bismuth layered compounds with extremely large crystal anisotropy are particularly suitable. Polymeric materials can also be used.
- raw materials such as CaCO, BaCO2, BiO, NbO, TaO, and TiO are used as starting materials.
- this calcined powder is again put into a ball mill and sufficiently wet-milled to produce a raw material powder mainly composed of a non-ferromagnetic substance. Then, an appropriate amount of a dispersant, water, and an organic binder are mixed with the raw material powder to prepare a slurry.
- the viscosity of the slurry is controlled to 30 to 200 mPa ′s by adjusting the blending ratio of the raw material powder and water.
- the viscosity of the slurry becomes less than 30 mPa's, the fluidity of the slurry increases, and it becomes difficult to maintain the orientation imparted in the first orientation imparting step described later, There is a possibility that the orientation is lowered.
- the viscosity of the slurry exceeds 200 mPa's, the viscosity of the slurry increases, making it difficult to orient the crystal axes regardless of the magnitude of the magnetic susceptibility. There is a risk of inviting.
- the viscosity of the slurry is controlled to be 30 to 200 mPa ⁇ s, preferably 60 to 11 OmPa ⁇ s.
- a first magnetic field is applied in the horizontal direction to the slurry accommodated in the slurry filling device (molding device), and the magnetic susceptibility to the magnetic field is The first crystal axis that is practically maximum is oriented in the direction in which the magnetic field is applied.
- a superconducting magnet as shown in FIG. 2 is prepared.
- the superconducting magnet 5 is formed in a cylindrical shape having a hollow portion 6, and a coil 7 is helically supported. When a voltage is applied to the superconducting magnet 5 to energize it, a magnetic field is generated in the direction of the arrow X (longitudinal direction). Although the superconducting magnet 5 is used in the present embodiment, a normal electromagnet can be used.
- a mud dripping device is arranged in the cavity 6 and a molding process is performed in a magnetic field.
- FIG. 3 is a schematic view of a mud dripping device, in which 8 is a saddle type and 9 is a porous absorbent plate.
- a mud dripping device is arranged in the cavity 6 of the superconducting magnet 5, and the superconducting magnet 5 is energized to generate a magnetic field in the direction of the arrow X.
- Slurry 10 is poured from the formed holes (not shown), and the slurry 10 is absorbed by the porous absorbent plate 9 to perform a forming process.
- the crystal grains of the slurry are oriented so that the first crystal axis having the maximum magnetic susceptibility is substantially in the magnetic field application direction.
- the other crystal axes are randomly oriented in any direction.
- the magnetic susceptibility of the crystal axis is a-axis> b-axis> c-axis
- the magnetic susceptibility of the a-axis becomes the susceptibility of the b-axis or c-axis. Therefore, the a-axis becomes the first crystal axis and is oriented in the direction of arrow X, which is the direction in which the magnetic field is applied.
- the b-axis and c-axis are randomly oriented in the plane perpendicular to the arrow X direction.
- the slurry 10 should not be vibrated. Rotate the mud grinder 90 ° horizontally. In this state, the superconducting magnet 5 is energized again to apply the second magnetic field, and a magnetic field is generated in the arrow X direction. As a result, the slurry 10 is applied in a direction perpendicular to the application direction in the first orientation imparting step 2, and the magnetic force is the maximum because the first orientation is maintained. Crystal axes other than the crystal axis of 1 are oriented.
- the & axis (first crystal axis) to which orientation was imparted in the first orientation imparting step 2 is perpendicular to the direction in which the second magnetic field is applied. Orientation is maintained in the direction facing the direction, and the b-axis has a higher magnetic susceptibility than the c-axis, so the b-axis is oriented in the arrow X direction. As a result, the c-axis is oriented in a third direction perpendicular to the first and second application directions.
- the slurry is dried for a predetermined time, whereby a non-ferromagnetic molded body is manufactured.
- the magnetic field having the maximum magnetic susceptibility is obtained by generating the magnetic field twice so that the application directions of the slurry prepared in the slurry preparation step 1 are perpendicular to each other and performing the forming process in the magnetic field.
- Orientation can also be imparted to crystal axes other than the crystal axis of 1.
- the orientation is imparted to crystal axes other than the crystal axis that has a substantially maximum magnetic susceptibility to a magnetic field.
- a magnetic material molded body can be produced.
- the second orientation imparting step 3 and the orientation fixing step 4 are performed separately. However, in the second orientation imparting step 3, the second magnetic field is applied. While applying, the second orientation imparting step 3 and the orientation fixing step 4 which may start drying may be performed simultaneously.
- the magnetic field is applied to the slurry 10 so as to be perpendicular to each other only by rotating the mud soaking apparatus. Therefore, the single superconducting magnet 5 is different. Two magnetic fields can be applied from the direction.
- the present invention is not limited to the above embodiment, and the magnitude of the applied magnetic field is preferably 1 T or more in order to obtain good orientation.
- the magnetic susceptibility of the crystal axis is a-axis> b-axis> c-axis.
- the magnetic susceptibility is a-axis axis> c-axis.
- orientation is imparted to one of the crystal axes (a axis or b axis) out of the crystal axes excluding the crystal axis having the minimum magnetic susceptibility (c axis).
- the a-axis is in contrast to the one in which the a-axis is oriented in the first orientation imparting step 2, and the a-axis to the one in which the b-axis is oriented.
- the c-axis having the minimum magnetic susceptibility is also necessarily oriented.
- the first orientation imparting step 1 and the second orientation imparting step 2 are performed continuously without providing a time interval.
- a fixed time interval may be provided between the orientation imparting step 2 and the orientation imparting step 2. That is, when a time interval is provided between the first orientation imparting step 1 and the second orientation imparting step 2, the first orientation imparting step 1 and the second orientation imparting step 2 Compared with the case where the steps are continuously performed, the orientation is slightly lowered, but the orientation of each crystal axis can be ensured.
- the first and second magnetic fields are applied in directions perpendicular to each other on the XY plane, but are applied in directions perpendicular to each other on the XZ plane. However, it may be applied so that the magnetic field is generated in a substantially vertical direction even if it is not truly vertical.
- the method of fixing the orientation of the crystal axis is not limited to the above-described drying treatment, but the orientation may be fixed by ultraviolet irradiation or the like.
- a slurry containing a non-ferromagnetic material having anisotropy in magnetic susceptibility is subjected to a molding process while applying a magnetic field.
- a non-ferromagnetic material molded body is a non-ferromagnetic material in which orientation is imparted to crystal axes other than the first crystal axis where the magnetic susceptibility of the crystal axis with respect to a magnetic field is substantially maximum.
- a molded product can be obtained.
- the non-ferromagnetic material is mainly composed of a bismuth layered compound
- a non-ferromagnetic material molded body in which orientation is imparted even to the c-axis having the smallest magnetic susceptibility can be obtained.
- the bismuth layered compound since the c-axis is the longest axis among the crystal axes, depending on the application, it is possible to provide a piezoelectric component having a large piezoelectric characteristic and displacement when an electric field is applied.
- the orientation fixing process is performed. It is common to use a ceramic molded body that has been solidified through baking to obtain a ceramic sintered body and then use it as a piezoelectric component body.
- a ceramic molded body that has been solidified through baking to obtain a ceramic sintered body and then use it as a piezoelectric component body.
- a polymer material is used, a non-ferromagnetic substance is used. It can also be used as it is.
- non-ferromagnetic material molded body When such a non-ferromagnetic material molded body is used as an electronic component, it is useful to use it as, for example, a semiconductor protective film, a printed circuit board, and an electromagnetic shielding material, but the present invention is not limited thereto. is not.
- the susceptibility of a-axis and b-axis is equally high.
- the susceptibility of c-axis is lower than the susceptibility of a-axis and b-axis.
- CaCO, Bi 2 O 3, TiO, and MnCO are prepared as starting materials.
- the starting materials were weighed so that
- this weighed product was put into a ball mill containing PSZ and mixed wet for about 16 hours. After the resulting mixture was dried, it was calcined at 1200 ° C for 2 hours. Then, using a rotary pulverizer, the powder was crushed in a dry process for 1 minute to obtain a calcined powder.
- the calcined powder is again put into the ball mill and subjected to a wet pulverization treatment for about 100 hours to obtain a raw material powder. Further, water and water are added to the raw material powder so as to have a blending amount as shown in Table 1.
- An organic binder (vinyl acetate resin) was mixed to prepare 6 types of ceramic slurries (Slurries A to F).
- the viscosities of the slurries A to F were measured with a vibratory viscometer.
- Table 1 shows the contents and viscosity in each slurry of raw material powder, water, and organic binder.
- the slurries A to F obtained in this way are poured into the bowl of the mud filling apparatus shown in FIG. 3, and the mud filling is put into the cavity 6 of the superconducting magnet 5 shown in FIG.
- the molding process was performed while applying a magnetic field by the magnetic field application method shown in (1) to (5) below.
- the ceramic molded body thus obtained was heat-treated at a temperature of 500 ° C for 2 hours to remove the organic binder, and then fired in the atmosphere at a temperature of 1200 ° C for 2 hours. Giving
- FIG. 4 shows the appearance of the ceramic sintered body
- P is the first magnetic field application direction
- Q is the first
- the second magnetic field application direction is shown.
- ⁇ I (HKL) is the sum of X-ray peak intensities of specific crystal planes (HKL) in the ceramic sintered body
- ⁇ I (hkl) is the total crystal plane (hkl) of the ceramic sintered body.
- X-ray peak intensity is the sum of X-ray peak intensities of specific crystal planes (HKL) of the above comparative powder sample
- ⁇ Io (hkl) is the total crystal plane (hkl) of the above comparative powder sample. This is the sum of X-ray peak intensities.
- Table 2 shows sample Nos. 1 to 18: Slurry No., magnetic field application method, crystal planes (100), (010), and (001) of planes A to C, and their respective degrees of orientation F1, F2, and electricity Mechanical coupling coefficient k Show.
- the degree of orientation is 0% in the case of non-orientation and 100% in the case where all crystal grains are oriented.
- Sample Nos. 3 and 4 are applying a magnetic field in the horizontal direction (direction of arrow P) to surface B. Therefore, the orientation degree of the a-axis and b-axis having a large magnetic susceptibility, that is, the orientation degree F1 of the (100) plane and the (010) plane, F1 is 71 to 78%.
- the degree of orientation of each crystal axis is as low as 6 to 16%, and the crystal axes are randomly oriented in any direction, and the electromechanical coupling coefficient k is also 12.:! ⁇ 12.4% was low.
- Sample Nos. 17 and 18 had an a-axis orientation on plane C where only the degree of orientation F1 on plane (100) and plane (010) of plane C was high at 67 to 76%.
- plane A and plane B the crystal axes are randomly oriented in any direction, so the degree of orientation in plane A and plane B is 7-14.
- the electromechanical coupling coefficient k was also low at 14.9-15.3% due to the low / 0 . This is sample number 17, 18
- sample numbers 5 to 16 applied a magnetic field in the direction of arrow Q perpendicular to the direction of arrow P after applying a magnetic field in the direction of arrow P.
- Orientation degree F1 of the plane and (010) plane is as high as 35 to 71%, and the orientation is given to the a axis, and in plane A, the orientation degree F2 of the (001) plane is 50 to 67% and the c axis Orientation is imparted, and therefore, orientation is imparted to any crystal axis, and the electromechanical coupling coefficient k is improved from 20. 0 to 23.0%.
- Sample numbers 11 to 15 Between the first magnetic field application and the second magnetic field application, such as
- the orientation of the c-axis on surface A was 50 to 55%, whereas the first magnetic field application and the second application as in sample numbers 5 to 10:
- the degree of orientation of the c-axis on surface A is as high as 57 to 63%. From these results, the first magnetic field application and the second magnetic field application Compared to the case where the magnetic field is continuously applied without a time interval, the orientation degree F 2 of the (001) plane in plane A can be increased, and a better electromechanical coupling coefficient k You can get a minute
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CN102303353A (zh) * | 2011-06-29 | 2012-01-04 | 浙江大学 | 运动磁场中梯度材料的凝胶注模制备方法 |
WO2012026397A1 (ja) * | 2010-08-26 | 2012-03-01 | 独立行政法人物質・材料研究機構 | 圧電セラミックスおよびその製造方法 |
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JP2002121069A (ja) * | 2000-10-10 | 2002-04-23 | Kyocera Corp | ビスマス層状化合物焼結体およびその製造方法 |
JP2005297556A (ja) * | 2004-03-16 | 2005-10-27 | Japan Science & Technology Agency | 一軸配向成型体の成型方法及びその成型装置 |
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JPH11513655A (ja) * | 1995-10-03 | 1999-11-24 | インダストリアル リサーチ リミテッド | 結晶材料の2つの軸を整列配向する方法 |
JP2002121069A (ja) * | 2000-10-10 | 2002-04-23 | Kyocera Corp | ビスマス層状化合物焼結体およびその製造方法 |
JP2005297556A (ja) * | 2004-03-16 | 2005-10-27 | Japan Science & Technology Agency | 一軸配向成型体の成型方法及びその成型装置 |
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WO2012026397A1 (ja) * | 2010-08-26 | 2012-03-01 | 独立行政法人物質・材料研究機構 | 圧電セラミックスおよびその製造方法 |
JPWO2012026397A1 (ja) * | 2010-08-26 | 2013-10-28 | 独立行政法人物質・材料研究機構 | 圧電セラミックスおよびその製造方法 |
CN102303353A (zh) * | 2011-06-29 | 2012-01-04 | 浙江大学 | 运动磁场中梯度材料的凝胶注模制备方法 |
CN102303353B (zh) * | 2011-06-29 | 2014-01-29 | 浙江大学 | 运动磁场中梯度材料的凝胶注模制备方法 |
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