US20080257472A1 - Method for manufacturing ceramic plates - Google Patents

Method for manufacturing ceramic plates Download PDF

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Publication number
US20080257472A1
US20080257472A1 US11/955,809 US95580907A US2008257472A1 US 20080257472 A1 US20080257472 A1 US 20080257472A1 US 95580907 A US95580907 A US 95580907A US 2008257472 A1 US2008257472 A1 US 2008257472A1
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Prior art keywords
ceramic
metal
layers
firing
green sheets
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US11/955,809
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Inventor
Hiroshi Asano
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Murata Manufacturing Co Ltd
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Murata Manufacturing Co Ltd
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Assigned to MURATA MANUFACTURING CO., LTD. reassignment MURATA MANUFACTURING CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ASANO, HIROSHI
Publication of US20080257472A1 publication Critical patent/US20080257472A1/en
Priority to US13/653,453 priority Critical patent/US8758536B2/en
Abandoned legal-status Critical Current

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    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
    • C04B37/006—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts consisting of metals or metal salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
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    • B32B2311/00—Metals, their alloys or their compounds
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    • B32B2311/08—Silver
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    • H05K3/1283—After-treatment of the printed patterns, e.g. sintering or curing methods
    • H05K3/1291—Firing or sintering at relative high temperatures for patterns on inorganic boards, e.g. co-firing of circuits on green ceramic sheets
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T156/1105—Delaminating process responsive to feed or shape at delamination
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T156/11—Methods of delaminating, per se; i.e., separating at bonding face
    • Y10T156/1111—Using solvent during delaminating [e.g., water dissolving adhesive at bonding face during delamination, etc.]

Definitions

  • the present invention relates to methods for manufacturing ceramic plates, and more particularly, relates to a method for manufacturing ceramic plates in which ceramic layers are separated from a sintered body including ceramic layers and metal layers alternately laminated to each other, to obtain the ceramic plates.
  • a method for forming thin ceramic plates has been proposed in which, after a laminate is formed by laminating ceramic green sheets provided with un-sintered metal films, the laminate is processed by a firing treatment to form a sintered body 103 composed of ceramic layers 101 and metal layers 102 alternately laminated to each other, and as shown in FIG. 13 , while the sintered body 103 is immersed in an alcohol 104 , an external force, such as ultrasonic waves, is applied to the sintered body 103 as shown by arrows to separate the metal layers 102 and the ceramic layers 101 .
  • preferred embodiments of the present invention provide a method for manufacturing ceramic plates, which can efficiently manufacture extremely thin ceramic plates without causing any damage thereto, and which can be easily applied to laminate type electronic components.
  • connection factors (1) to (4) when the above connection factors (1) to (4) are all removed, without applying any external force to the sintered body, the ceramic layer and the metal layer can be easily separated from each other.
  • connection factors (1) to (4) described above oxygen present between the ceramic layer and the metal layer can be removed when the sintered body is immersed in an oxygen removal processing liquid so as to cause an oxidation-reduction reaction at the interface; the factor (2) can be resolved when an unsintered metal film is formed to have a large thickness such that crosslinking does not occur between the ceramic layers; the factor (3) can be resolved when a metal material which does not diffuse into the ceramic layer side during a firing treatment is used; and as for the factor (4), when the firing temperature is set to a high temperature at which no glass component remains on a surface of the ceramic layer after firing and to a temperature equal to or lower than a decomposition temperature of a ceramic material forming the ceramic layer, even after the laminate is processed by the firing treatment, the glass component can be prevented from remaining on the surface of the ceramic layer without decomposition of the ceramic material.
  • a method for manufacturing ceramic plates according to a preferred embodiment of the present invention is a method for manufacturing ceramic plates by separating ceramic layers from a sintered body composed of the ceramic layers and metal layers alternately laminated to each other, and the method includes: a ceramic green-sheet forming step of forming ceramic green sheets from ceramic raw materials; a metal paste forming step of forming a metal paste using a metal component as a solid component which does not diffuse into the ceramic during firing; a metal film forming step of applying the metal paste on surfaces of the ceramic green sheets to form metal films each having a thickness such that ceramic layers to be formed after firing are not connected to each other in the lamination direction; a laminate forming step of laminating the ceramic green sheets provided with the metal films to form a laminate; a firing step of performing a firing treatment for the laminate at a firing temperature which is set to a high temperature at which no glass component remains on surfaces of the ceramic layers after the firing and to a temperature equal to or
  • the method for manufacturing ceramic plates may further include: an electrode paste forming step of forming an electrode paste containing a conductive component which diffuses into the ceramic green sheets during the firing; and an electrode film forming step of applying the electrode paste on surfaces of the ceramic green sheets to form electrode films, and in addition, the laminate formed in the laminate forming step includes the ceramic green sheets provided with the electrode films.
  • palladium may be used as the metal component which does not diffuse into the ceramic during the firing.
  • the metal component of the metal paste may include palladium.
  • a reducing solution including an organic compound which includes at least one of a hydroxyl group (—OH), an aldehyde group (—CHO), and a carboxyl group (—COOH) may be used; in particular, a liquid alcohol is preferably used which is one of an aliphatic alcohol, a cycloaliphatic alcohol, an aromatic alcohol, a heterocyclic alcohol, and a mixture thereof; and as the liquid alcohol, in particular, as the aliphatic alcohol, n-butyl alcohol is more preferably used.
  • the oxygen removal processing liquid may be a reducing solution which includes an organic compound containing at least one of a hydroxyl group, an aldehyde group, and a carboxyl group.
  • the oxygen removal processing liquid may comprise a liquid alcohol
  • the liquid alcohol may be one of an aliphatic alcohol, a cycloaliphatic alcohol, an aromatic alcohol, a heterocyclic alcohol, and a mixture thereof.
  • the aliphatic alcohol is preferably n-butyl alcohol.
  • preferred embodiments of the present invention are suitable for use to obtain ceramic plates of a lead-based piezoelectric ceramic material.
  • the ceramic material forming the ceramic green sheets is preferably a lead-based piezoelectric ceramic material containing a lead component.
  • the thickness of the metal film which prevents the ceramic layers to be formed by the firing from being connected to each other in the lamination direction varies depending on ceramic materials to be used, it was discovered that from the results of the research carried out by the inventors of the present invention, in the case in which a piezoelectric ceramic material is used, when the thickness of the metal film is set in the range of about 1.9 ⁇ m to about 10 ⁇ m, for example, the ceramic layers can be formed so as not to be connected to each other.
  • the thickness of the metal film is preferably in the range of about 1.9 ⁇ m to about 10 ⁇ m, for example.
  • the ceramic green-sheet forming step may form a plurality types of ceramic green sheets which have different thicknesses.
  • the method for manufacturing ceramic plates includes: a ceramic green-sheet forming step of forming ceramic green sheets from ceramic raw materials; a metal paste forming step of forming a metal paste using a metal component (such as palladium) as a solid component which does not diffuse into ceramic during firing; a metal film forming step of applying the metal paste on surfaces of the ceramic green sheets to form metal films each having a thickness (such as about 1.9 ⁇ m to about 10 ⁇ m) so that ceramic layers to be formed after firing are not connected to each other; a laminate forming step of laminating the ceramic green sheets provided with the metal films to form a laminate; a firing step of performing a firing treatment for the laminate at a firing temperature which is set to a high temperature at which no glass component remains on surfaces of the ceramic layers to be formed after the firing and to a temperature equal to or lower than a decomposition temperature of a ceramic material, such as a lead-based piezoelectric ceramic material, forming the ceramic layers so as to form the
  • the method for manufacturing ceramic plates may further include an electrode paste forming step of forming an electrode paste containing a conductive component which diffuses into the ceramic during the firing and an electrode film forming step of applying the electrode paste on surfaces of the ceramic green sheets to form electrode films
  • the laminate formed in the laminate forming step may include the ceramic green sheets provided with the electrode films, when the ceramic green sheets provided with the electrode films and the ceramic green sheets provided with the metal films are appropriately laminated to each other, ceramic layers each having a laminate structure composed of the ceramic layers and the electrode layers, which are alternately laminated to each other, can be separated from the metal layers. Accordingly, the ceramic layers each having the laminate structure described above can be used as ceramic plates and can be easily applied to laminate type electronic components.
  • the ceramic green-sheet forming step may form a plurality types of ceramic green sheets which have different thicknesses, ceramic layers having different thicknesses can be separated from the metal layers, and hence ceramic plates having different thicknesses can be simultaneously and easily manufactured.
  • FIG. 1 is a flowchart of a method for manufacturing ceramic plates of a preferred embodiment according to the present invention.
  • FIG. 2 is a cross-sectional view showing the state in which metal films are formed on ceramic green sheets in a metal film forming step.
  • FIG. 3 is a view illustrating a problem in the case in which a metal film has a small thickness.
  • FIG. 4 is a cross-sectional view of a sintered body obtained in a sintering step.
  • FIG. 5 is a view showing the state in which a sintered body is immersed in an oxygen removal processing liquid in a separation step.
  • FIG. 6 is a cross-sectional view showing the state in which ceramic layers and metal layers are separated from each other.
  • FIG. 7 is a flowchart of a method for manufacturing ceramic plates of another preferred embodiment according to the present invention.
  • FIG. 8 is a cross-sectional view of a sintered body obtained in a sintering step of another preferred embodiment of the present invention.
  • FIG. 9 is a cross-sectional view showing the state in which ceramic layers each having a laminate structure and metal layers are separated from each other.
  • FIG. 10 is a cross-sectional view of a first laminate formed in Example 6.
  • FIG. 11 is a cross-sectional view of a second laminate formed in Example 6.
  • FIG. 12 is a cross-sectional view of a third laminate formed in Example 6.
  • FIG. 13 is a view showing a conventional method for manufacturing ceramic plates.
  • FIG. 1 is a flowchart showing a method for manufacturing ceramic plates of a preferred embodiment according to the present invention, and hereinafter, the case in which ceramic plates containing a Pb component are manufactured will be described.
  • ceramic green sheets are formed from ceramic raw materials.
  • ceramic raw materials such as Pb 3 O 4 , TiO 2 , and ZrO 2
  • predetermined amounts are weighed and charged in a ball mill containing pulverizing media, followed by mixing and wet pulverization, drying is performed, and a calcination treatment is then performed at a predetermined temperature, so that a powdered piezoelectric ceramic is formed.
  • an organic binder and a dispersing agent are added to the powdered piezoelectric ceramic together with purified water and are then again mixed and wet-pulverized in a ball mill to form a ceramic slurry, and subsequently, the ceramic slurry is processed by a forming method such as a doctor blade method, thereby forming ceramic green sheets each having a predetermined thickness.
  • a metal paste to be applied to surfaces of the ceramic green sheets is formed.
  • a metal component such as powdered Pd (palladium), which does not diffuse into ceramic during firing is mixed with an organic vehicle and is then compounded therewith using a three-roller mill to form the metal paste.
  • a compound may be used which is formed of an organic solvent, such as terpineol, and an organic binder, such as an ethyl cellulose resin, dissolved therein.
  • the ratio between the Pd powder and the organic vehicle is not particularly limited; however, for example, a compound containing powdered Pd and an organic vehicle at a ratio of about 55% to about 45% on a weight percent basis may be used.
  • a metal film forming step 3 as shown in FIG. 2 , the metal paste is applied to the entire surfaces of ceramic green sheets 7 a to 7 d to form metal films 8 a to 8 d.
  • the ceramic green sheets 7 a to 7 d provided with the metal films 8 a to 8 d, respectively, are laminated to each other and are then fired as described below, when the thicknesses of the metal films 8 a to 8 d are small, for example as shown in FIG. 3 , holes are formed in a metal layer 10 a ′ which is a sintered body of the metal film 8 a, and the holes are filled with a ceramic material.
  • a metal layer 10 a ′ which are sintered bodies of the ceramic green sheets 7 a and 7 b, respectively, are connected to each other through the metal layer 10 a ′, and crosslinking 10 a ′′ is formed. Accordingly, since the ceramic layers are tightly connected to each other by the crosslinking 10 a ′′ interposed therebetween, it becomes difficult to separate the ceramic layers 9 a and 9 b from the metal layer 10 a′.
  • the thicknesses of the metal films 8 a to 8 d are adjusted so that the ceramic layers to be formed after the firing are not connected to each other.
  • the desired thickness of the metal film 8 as described above varies depending on ceramic materials. However, in the case in which a Pb-based piezoelectric ceramic is used as this preferred embodiment, the thickness is preferably in the range of about 1.9 ⁇ m to about 10 ⁇ m and is more preferably in the range of about 3 ⁇ m to about 5 ⁇ m, for example.
  • a firing treatment is performed for the laminate described above, and as shown in FIG. 4 , a sintered body 11 composed of ceramic layers 9 ( 9 a to 9 e ) and metal layers 10 ( 10 a to 10 d ) alternately laminated to each other is formed.
  • the firing temperature is set to a high temperature at which no glass component remains on surfaces of the ceramic layers 9 and is also set to a temperature equal to or lower than a decomposition temperature of a ceramic material forming the ceramic layers 9 .
  • liquid phase PbO is generally generated when a firing treatment is performed
  • liquid phase PbO also permeates the interfaces between the metal films 8 and the respective ceramic green sheets 7 during the firing treatment, when the sintering is completed in the state described above, low melting point glass layers are formed at the interfaces between the metal layers 10 which are sintered bodies of the metal films 8 and the respective ceramic layers 9 which are sintered bodies of the ceramic green sheets 7 . That is, the glass component remains on the surfaces of the ceramic layers 9 .
  • the glass component described above functions as an adhesive to the metal layers 10 , a separation treatment, which will be described later, between the ceramic layers 9 and the respective metal layers 10 will be disturbed.
  • the firing temperature is set to a high temperature so that no glass component remains, and in this embodiment, the firing temperature is preferably set to about 1,100° C. or more.
  • the upper limit of the firing temperature must be set to the decomposition temperature of the ceramic material or less.
  • a separation step 6 as shown in FIG. 5 , the sintered body 11 is immersed in a treatment bath 13 filled with an oxygen removal processing liquid 12 , and as shown in FIG. 6 , the ceramic layers 9 and the metal layers 10 are separated from each other, so that the ceramic plates are obtained.
  • the connection factor between the ceramic layers 9 and the respective metal layers 10 is only oxygen present at the interfaces therebetween.
  • the sintered body 11 is immersed in the oxygen removal processing liquid 12 for a predetermined time, so that the oxygen present at the interfaces is removed.
  • a reducing solution of an organic compound including at least one of a hydroxyl group, an aldehyde group, and a carboxyl group may be used, and when the sintered body 11 is immersed in this type of reducing solution, an oxidation-reduction reaction occurs at the interface, so that the oxygen present at the interfaces can be removed.
  • a liquid alcohol is preferably used.
  • the liquid alcohol one of an aliphatic alcohol, a cycloaliphatic alcohol, an aromatic alcohol, a heterocyclic alcohol, and a mixture thereof may be used.
  • the method for manufacturing ceramic plates described above includes: the ceramic green-sheet forming step 1 of forming the ceramic green sheets 7 from the ceramic raw materials; the metal paste forming step 2 of forming the metal paste using Pd as a solid component which does not diffuse into ceramic green sheet 7 sides during firing; the metal film forming step 3 of applying the metal paste on the surfaces of the ceramic green sheets to form the metal films 8 each having a thickness such that the ceramic layers to be formed after firing are not connected to each other; the laminate forming step 4 of laminating the ceramic green sheets 7 provided with the metal films 8 to form a laminate; the firing step 5 of performing a firing treatment for the laminate at a firing temperature which is set to a high temperature at which no glass component remains on the surfaces of the ceramic layers 9 to be formed after the firing and to a temperature equal to or lower than the decomposition temperature of the Pb-based piezoelectric ceramic material so as to form the sintered body 11 composed of the ceramic layers 9 and the metal layers 10 alternately laminated to each other; and the separation step 6 of immersing the sin
  • the ceramic layers 9 and the metal layers 10 can be easily separated from each other, and as a result, good quality ceramic plates having no damage, such as cracks, can be obtained with high efficiency.
  • FIG. 7 is a flowchart showing a method for manufacturing ceramic plates of another preferred embodiment according to the present invention, and in this additional preferred embodiment, electrode films which diffuse into ceramic during firing are provided between ceramic green sheets, so that ceramic plates each having a laminate structure are obtained.
  • a conductive component such as Ag—Pd or Ag
  • a ceramic green sheet is laminated on the topmost layer, followed by pressure bonding, so that the laminate is formed.
  • a firing step 24 at a firing temperature which is set under temperature conditions similar to those of the above-described preferred embodiment, the laminate is processed by a firing treatment, so that a sintered body 40 containing a ceramic layer 26 a, an electrode layer 27 a, a ceramic layer 26 b, a metal layer 28 a, . . . and a ceramic layer 26 f laminated in that order as shown in FIG. 8 is obtained.
  • the sintered body 40 is immersed in the oxygen removal processing liquid used in the above-described preferred embodiment for a predetermined time. Since a portion of the conductive component forming the electrode layers 27 ( 27 a to 27 c ) diffuses to the ceramic layers 26 ( 26 a to 26 e ), the electrode layers 27 ( 27 a to 27 c ) are tightly connected to and are not separated from the ceramic layers 26 ( 26 a to 26 e ) which are in contact therewith so as to maintain laminate structures 29 ( 29 a to 29 c ), and in addition, the other side surfaces of the ceramic layers 26 b, 26 c, 26 d, and 26 e which are in contact with the metal layers 28 a and 28 b are separated therefrom, so that ceramic plates having laminate structures 29 a to 29 c can be obtained.
  • the ceramic plates each having a laminate structure can also be obtained and can be applied to laminate type electronic components having a laminate structure.
  • the present invention is not limited to the preferred embodiments described above, and without departing from the spirit and the scope of the present invention, various modifications may be made.
  • various ceramic green sheets having different thicknesses when various ceramic green sheets having different thicknesses are formed, various ceramic plates having different thicknesses can be easily obtained with high efficiency.
  • the Pb-based piezoelectric ceramic material is preferably used as a ceramic material, of course, another ceramic material, such as a non-lead piezoelectric ceramic material or a dielectric ceramic material, may also be used.
  • the ceramic green sheets provided with the electrode films and the ceramic green sheets provided with the metal films preferably are alternately laminated to each other, of course, the structure may be formed in which ceramic green sheets provided with the electrode films are laminated to each other, and on one surface in the above laminate at which the separation is desirably performed, a ceramic green sheet provided with the metal film may be provided.
  • this ceramic slurry was processed by a doctor blade method to form a ceramic green sheet having a thickness of about 20 ⁇ m, and this ceramic green sheet was then cut into sheets having a length of about 20 mm and a width of about 30 mm.
  • Pd paste a metal paste (hereinafter referred to as “Pd paste”) containing Pd as a solid component was formed.
  • this Pd paste was applied to the entire surfaces of the ceramic green sheets obtained by the above cutting step while the thickness thereof was being adjusted to about 3.0 ⁇ m, so that metal films were formed on the ceramic green sheets.
  • the firing treatment was performed for approximately 2 hours at temperatures different by about 20° C. in the range of from about 1,060 to about 1,180, and as a result, seven types of samples processed at the different firing temperatures were obtained (Sample No. 1).
  • first Ag—Pd paste having a composition ratio of Ag to Pd of about 70 to about 30 on a weight percent basis
  • second Ag—Pd paste an electrode paste having a composition ratio of Ag to Pd of about 30 to about 70 on a weight percent basis
  • Table 1 shows the status of separation at the individual temperatures.
  • O indicates the case in which the ceramic layer and the metal layer are completely separated from each other
  • ⁇ indicates the case in which the metal layer is partly adhered to one surface of the ceramic layer and cannot be completely separated therefrom.
  • X indicates the case in which the ceramic layer cannot be separated from the metal layer at all.
  • the ceramic layer and the metal layer could be separated from each other by increasing the intensity of the ultrasonic waves or by increasing the time for applying the ultrasonic waves; however, it was confirmed that cracks were generated in the separated ceramic layer, that is, in the ceramic plate.
  • a Pb ⁇ (Ni,Nb)Zr,Ti ⁇ O 3 -based piezoelectric ceramic powder was formed by a method and a procedure similar to those of Example 1 using Pb 3 O 4 , TiO 2 , ZrO 2 , NiO, and Nb 2 O 5 as ceramic raw materials.
  • Example 2 Subsequently, after samples of Sample Nos. 11 to 16 were formed in a manner similar to that in Example 1, were then immersed in a treatment bath filled with n-butyl alcohol for approximately 50 hours, and were then recovered from the treatment bath, whether the metal layer and the ceramic layer were separated or not was investigated.
  • the firing temperature was set to approximately 1,050° C., 1,110° C., 1,150° C., and 1,180° C.
  • Table 2 shows the status of separation at the individual firing temperatures.
  • o indicates the case in which the ceramic layer and the metal layer are completely separated from each other
  • x indicates the case in which the ceramic layer cannot be separated from the metal layer at all.
  • a (Pb,La)TiO 3 -based piezoelectric ceramic powder was formed by a method and a procedure similar to those of Example 1 using Pb 3 O 4 , TiO 2 , and La 2 O 3 as ceramic raw materials.
  • Metal films were formed by applying a Pd paste on surfaces of the ceramic green sheets formed in Example 1 so as to have thicknesses as shown in Table 3. Subsequently, samples of Sample Nos. 21 to 24 were obtained by a method and a procedure similar to those of Example 1 except that the firing was performed at a constant firing temperature of about 1,110° C.
  • the samples were immersed in n-butyl alcohol for approximately 50 hours, and the separation properties between the ceramic layer and the metal layer was investigated.
  • the thickness of the metal film was about 1.9 ⁇ m or more, good separation properties could be obtained between the metal layer and the ceramic layer.
  • the Pd paste, and the first Ag—Pd paste, which were formed in Example 1 were prepared, the Pd paste or the first Ag—Pd paste was applied on surfaces of the ceramic green sheets, so that the metal films or the electrode films were formed on the ceramic green sheets.
  • a sintered body was obtained by a method and a procedure similar to those of Example 1 except that the firing was performed at a constant firing temperature of about 1,120° C.
  • first ceramic green sheets having a thickness of about 10 ⁇ m and second ceramic green sheets having a thickness of about 100 ⁇ m were formed, and metal films having a thickness of about 3 ⁇ m were then formed on surfaces of the first and the second ceramic green sheets.
  • a second laminate was formed in which the first ceramic green sheets 30 a and 30 b provided with the metal films 31 a and 31 b, respectively, were sandwiched by a second ceramic green sheet 32 a provided with a metal film 33 a and a second ceramic green sheet 32 b provided with no metal film, those having a thickness larger than that of the first ceramic green sheets 30 a and 30 b, and a firing treatment similar to that described above was performed, thereby forming a second sintered body.
  • the first ceramic green sheet 30 a provided with the metal film 31 a was sandwiched by the second ceramic green sheets 32 a and 32 b provided with the metal film 33 a and a metal film 33 b, respectively, and having a thickness larger than that of the first ceramic green sheet 30 a, and on the topmost surface, the first ceramic green sheet 30 b was laminated to form a third laminate, followed by a firing treatment similar to that described above, so that a third sintered body was obtained.
  • the first to the third sintered bodies were immersed in n-butyl alcohol for approximately 50 hours, and it was confirmed that the ceramic layers and the metal layers were completely separated from each other.

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Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:ASANO, HIROSHI;REEL/FRAME:020242/0491

Effective date: 20071213

STCB Information on status: application discontinuation

Free format text: ABANDONED -- FAILURE TO PAY ISSUE FEE