Patent Grant
8716924
The present invention relates to a spark plug for an internal combustion engine.
A spark plug for providing ignition in an internal combustion engine, such as a gasoline engine, has the following structure: an insulator is provided externally of a center electrode; a metallic shell is provided externally of the insulator; and a ground electrode which forms a spark discharge gap in cooperation with the center electrode is attached to the metallic shell. The metallic shell is generally formed from an iron-based material, such as carbon steel, and, in many cases, plating is performed on its surface for corrosion protection. A known technique associated with such a plating layer employs a 2-layer structure consisting of an Ni plating layer and a chromate layer (See Japanese Patent Application Laid-Open (kokai) No. 2002-184552). However, the inventors of the present invention have found that, even in employment of a plating layer having such a two- or more-layer structure, corrosion resistance is still a big problem for a portion of a spark plug which is deformed at the time of crimping. The following description first discusses an example structure of a spark plug and a crimping step, and then a portion of the spark plug which is deformed from crimping and involves a problem with respect to corrosion resistance.
The insulator 2 is formed from, for example, a ceramic sintered body of alumina or aluminum nitride and has a through hole 6 formed therein in such a manner as to extend along the axial direction thereof, and adapted to allow the center electrode 3 to be fitted therein. A metal terminal 13 is fixedly inserted into the through hole 6 at a side toward one end of the through hole 6, whereas the center electrode 3 is fixedly inserted into the through hole 6 at a side toward the other end of the through hole 6. A resistor 15 is disposed, within the through hole 6, between the metal terminal 13 and the center electrode 3. Opposite end portions of the resistor 15 are electrically connected to the center electrode 3 and the metal terminal 13 via electrically conductive glass seal layers 16 and 17, respectively.
The metallic shell 1 is formed into a hollow, cylindrical shape from a metal, such as carbon steel, and forms a housing of the spark plug 100. The metallic shell 1 has a threaded portion 7 formed on its outer circumferential surface and adapted to mount the spark plug 100 to an unillustrated engine block. A hexagonal portion 1e is a tool engagement portion which allows a tool, such as a spanner or a wrench, to be engaged therewith in mounting the metallic shell 1 to the engine block, and has a hexagonal cross section. The tool engagement portion may have any cross-sectional shape (orthogonal-to-axis sectional shape) other than a hexagonal shape; for example, the tool engagement portion may have another polygonal cross section, such as an octagonal cross section. In a space between the outer surface of the insulator 2 and the inner surface of a rear (upper in the drawing) opening portion of the metallic shell 1, a ring packing 62 is disposed on the rear periphery of a flange-like projection 2e of the insulator 2, and a filler layer 61, such as talc, and a ring packing 60 are disposed, in this order, rearward of the ring packing 62. In assembling work, the insulator 2 is pressed forward (downward in the drawing) into the metallic shell 1, and, in this condition, the rear opening end of the metallic shell 1 is crimped inward toward the ring packing 60 (and, in turn, toward the projection 2e, which functions as a receiving portion for crimping), whereby a crimp portion 1d is formed, and thus the metallic shell 1 is fixed to the insulator 2.
A gasket 30 is fitted to a proximal end of the threaded portion 7 of the metallic shell 1. The gasket 30 is formed by bending a metal sheet of carbon steel or the like into the form of a ring. When the threaded portion 7 is screwed into a threaded hole of the cylinder head, the gasket 30 is compressed in the axial direction and deformed in a crushed manner between a flange-like gas seal portion 1f f of the metallic shell 1 and a peripheral-portion-around-opening of the threaded hole, thereby sealing the gap between the threaded hole and the threaded portion 7.
Then, as shown in
According to the above-mentioned conventional technique (See Japanese Patent Application Laid-Open (kokai) No. 2002-184552), an electrolytic chromating process is performed such that 95% by mass or more of the chromium component of a chromate layer is trivalent chromium. The purpose of such chromating is to reduce environmental burden through attainment of substantially zero content of hexavalent chromium and to improve corrosion resistance against salt water (salt corrosion resistance).
However, as mentioned above, crimping causes the crimp portion 1d and the groove portion 1h to be greatly deformed, resulting in the generation of a large residual stress in these portions; therefore, corrosion resistance is a big problem for these portions. That is, the crimp portion 1d and the groove portion 1h are characterized by the presence of a large residual stress caused by crimping-induced deformation. Particularly, in the case of employment of hot crimping, hardness increases as a result of a change of microstructure associated with application of heat. A portion which has such high hardness and in which a large residual stress exists may suffer stress corrosion cracking. The inventors of the present invention have found that, particularly in a spark plug, not only salt corrosion resistance, but also stress corrosion cracking resistance is a big problem to consider for the crimp portion 1d and the groove portion 1h. Such a problem to consider is particularly marked in a case of using the metallic shell formed from a material having a high content of carbon (e.g., carbon steel which contains carbon in an amount of 0.15% by weight or more). Such a problem to consider is also marked in the case of employing hot crimping.
Conventionally employed nickel plating specifications give importance to corrosion resistance of the outer surface of the metallic shell and tend to not give much importance to the plating thickness of the inner surface. However, since the inner surface of the metallic shell is in a closed space, dew condensation is apt to occur thereon upon exposure to coldness. Also, since the inner surface is thin in plating thickness as compared with the outer surface, the occurrence of stress corrosion cracking associated with progress of corrosion is more concerned. In view of these findings and consideration, the inventors of the present invention have reached the understanding that it is important to design the plating thickness of the inner surface of the metallic shell to restrain stress corrosion cracking, and thus have conceived the present invention.
Generally, if a plating thickness of the same level is ensured for the inner and outer surfaces of the metallic shell (if the inner surface can be coated with sufficiently thick plating), sufficient stress corrosion cracking resistance conceivably can be ensured. However, in actuality, the following has been found: when plating on the inner surface is excessively thick, crimping-induced deformation causes cracking to occur in the plating on the inner surface, resulting in deterioration in stress corrosion cracking resistance. Therefore, importantly, the plating thickness of the inner surface must fall within such an appropriate range as not to lead to the occurrence of cracking after crimping. That is, in designing nickel plating on the metallic shell, preferably, the nickel plating thickness of the inner surface is determined so as to be appropriate to stress corrosion cracking resistance. Particularly, desirably, the nickel plating thickness of the outer surface and the nickel plating thickness of the inner surface are specified in such a balanced manner that the nickel plating thickness of the outer surface is appropriate to corrosion resistance, whereas the nickel plating thickness of the inner surface is appropriate to stress corrosion cracking resistance.
An object of the present invention is to provide a spark plug to which excellent stress corrosion cracking resistance is imparted by means of appropriately specifying the nickel plating thickness of the inner surface of the metallic shell.
The present invention has been conceived to solve, at least partially, the above problems and can be embodied in the following modes or application examples.
Application example 1 A spark plug comprising:
Application example 2 A spark plug comprising:
Application example 3 A spark plug comprising:
Application example 4 A spark plug comprising:
Application example 5 A spark plug according to any one of application examples 1 to 4, wherein, as measured on an outer surface of the tool engagement portion, the nickel plating layer has a thickness of 3 μm to 15 μm.
Application example 6 A spark plug according to any one of application examples 1 to 5, wherein the metallic shell and an insulator accommodated in the metallic shell are fitted together by hot crimping.
Application example 7 A spark plug according to any one of application examples 1 to 6, wherein the groove portion has a height of 3.5 mm to 6.5 mm as measured in the axial direction.
The present invention can be embodied in various forms. For example, the present invention can be embodied in a spark plug, a metallic shell for the spark plug, a method of manufacturing the spark plug, and a method of manufacturing the metallic shell.
The configuration of application example 1 can provide a spark plug having excellent stress corrosion cracking resistance by means of employing a nickel plating layer thickness of 0.3 μm to 2.0 μm as measured at the forward end of the inner circumferential surface of the groove portion of the metallic shell.
The configuration of application example 2 can provide a spark plug having excellent stress corrosion cracking resistance in the case where the chromium-containing layer is formed on the nickel plating layer of the metallic shell, by means of employing a nickel plating layer thickness of 0.2 μm to 2.2 μm as measured at the forward end of the inner circumferential surface of the groove portion of the metallic shell.
The configuration of application example 3 can provide a spark plug having excellent stress corrosion cracking resistance in the case where rust prevention oil is applied onto the nickel plating layer of the metallic shell, by means of employing a nickel plating layer thickness of 0.2 μm to 2.2 μm as measured at the forward end of the inner circumferential surface of the groove portion of the metallic shell.
The configuration of application example 4 can provide a spark plug having excellent stress corrosion cracking resistance in the case where the chromium-containing layer is formed on the nickel plating layer of the metallic shell, and rust prevention oil is applied onto the chromium-containing layer, by means of employing a nickel plating layer thickness of 0.1 μm to 2.4 μm as measured at the forward end of the inner circumferential surface of the groove portion of the metallic shell.
The configuration of application example 5 can provide a spark plug having not only excellent stress corrosion cracking resistance but also excellent corrosion resistance (salt corrosion resistance) and plating peeling resistance.
The configuration of application example 6 can provide a spark plug having excellent stress corrosion cracking resistance even in the case where hot-crimping-induced deformation puts stress corrosion cracking resistance at stake, by means of employing a nickel plating layer thickness in the above-mentioned appropriate ranges as measured at the forward end of the inner circumferential surface of the metallic shell.
Generally, as the opposite side-to-side dimension of the tool engagement portion (for example, the distance between opposite sides of the hexagonal portion) reduces (for example, 14 mm or less), the height (length in the axial direction) of the groove portion must be increased in order to ensure gastightness. This is for the following reason: increasing the height of the groove portion allows an increase in the amount of deformation of the groove portion at the time of crimping, whereby fixation can be further enhanced. According to the configuration of application example 7, the height of the groove portion is 3.5 mm or more; thus, the amount of deformation of the groove portion is increased. Accordingly, stress corrosion cracking is more likely to occur; therefore, the effect of the present invention of preventing stress corrosion cracking is more markedly produced. Meanwhile, when the height of the groove portion is in excess of 6.5 mm, the deformation of the groove portion is excessively increased; therefore, the effect of preventing stress corrosion cracking is limited.
a)-2(d) are explanatory views showing an example crimping step of fixing a metallic shell to an insulator.
A spark plug according to an embodiment of the present invention has the configuration shown in
Example of Processing Conditions of Nickel Strike Plating
Composition of plating bath
Processing temperature (bath temperature): 25-40° C.
Cathode current density: 0.2-0.4 A/dm2
Processing time: 5-20 minutes
In step T110, an electrolytic nickel plating process is performed. The electrolytic nickel plating process can be a barrel-type electrolytic nickel plating process which uses a rotary barrel, and may employ another plating method, such as a stationary plating method. Usually employed processing conditions can be employed for electrolytic nickel plating. A specific example of preferable processing conditions is as follows.
Example of Processing Conditions of Electrolytic Nickel Plating
Composition of plating bath
Bath pH: 2.0-4.8
Processing temperature (bath temperature): 25-60° C.
Cathode current density: 0.02-3.0 A/dm2
Processing time: 5-600 minutes
The lower the cathode current density, the smaller the difference in Ni plating layer thickness between the outer surface and the inner surface of the metallic shell, and, the higher the cathode current density, the larger the difference. Meanwhile, the longer the processing time, the greater the Ni plating layer thickness. Therefore, the balance of the Ni plating layer thickness between the outer surface and the inner surface of the metallic shell can be adjusted by adjusting a combination of the cathode current density and the processing time.
In step T120, if necessary, an electrolytic chromating process is performed, thereby forming a chromate layer (also called the “chromium-containing layer”). The electrolytic chromating process can also use a rotary barrel and may employ another plating method, such as a stationary plating method. An example of preferable processing conditions of the electrolytic chromating process is as follows.
Example of Processing Conditions of Electrolytic Chromating Process
Composition of processing bath (chromating processing solution)
Bath pH: 2-6
Processing temperature (bath temperature): 20-60° C.
Cathode current density: 0.02-0.45 A/dm2
Processing time: 1-10 minutes
A usable dichromate other than sodium dichromate is potassium dichromate. Another combination of processing conditions (amount of dichromate, cathode current density, processing time, etc.) different from the above may be employed according to a desired thickness of the chromate layer. This electrolytic chromating process is an electrolytic trivalent chromating process in which the chromium component in the chromate layer is trivalent chromium. Preferable processing conditions of the chromating process will be described later together with experimental results.
When the Ni plating process and the electrolytic chromating process are performed, a film of 2-layer structure consisting of the nickel plating layer and the chromate layer is formed on the outer and inner surfaces of the metallic shell. However, the electrolytic chromating process can be omitted. Also, still another protection film may be formed on the 2-layer structure consisting of the nickel plating layer and the chromate layer.
In step T130, if necessary, rust prevention oil is applied as a protection film. Commercially available various rust prevention oils can be used. Rust prevention oil can be applied, for example, by immersing the entire metallic shell in rust prevention oil. Usable rust prevention oil contains at least one of C (mineral oil), Ba, Ca, Na, and S. If the Ba content is excessively high, the appearance of the metallic shell may discolor. As for the components other than Ba, if their contents are excessively low, corrosion resistance may deteriorate, and, if their contents are excessively high, nonuniform color tone or discoloration may occur after application of rust prevention oil. Application of rust prevention oil can be omitted.
After various protection films are formed as mentioned above, the metallic shell is fixed to the insulator, etc., by the crimping step, thereby completing the spark plug. In addition to cold crimping, hot crimping can also be used in the crimping step.
In the first example, there were manufactured a plurality of metallic shell samples which differed in the Ni plating thickness of the inner surface by executing step T100 (Ni strike plating process) and step T110 (electrolytic Ni plating process) of
First, the metallic shells 1 were manufactured, by cold forging, from a carbon steel wire SWCH17K for cold forging specified in JIS G3539. The ground electrodes 4 were welded to the respective metallic shells 1, followed by degreasing and water washing. Subsequently, a nickel strike plating process was performed under the following processing conditions by use of a rotary barrel.
Processing Conditions of Nickel Strike Plating
Composition of plating bath
Processing temperature (bath temperature): 30° C.
Cathode current density: 0.3 A/dm2
Processing time: 15 minutes
Next, an electrolytic nickel plating process was performed under the following processing conditions by use of the rotary barrel, thereby forming nickel plating layers.
Processing Conditions of Electrolytic Nickel Plating
Composition of plating bath
Bath pH: 4.0
Processing temperature (bath temperature): 55° C.
Cathode current density: 0.03-2.4 A/dm2
Processing time: 5-600 minutes
We can read, from
In order to evaluate stress corrosion cracking resistance, the following accelerated corrosion test was conducted. Four holes each having a diameter of about 2 mm were cut in the groove portions 1h of the samples (metallic shells); subsequently, the insulators, etc., were fixed by crimping. The holes were cut for allowing entry of a corrosive solution for test into the metallic shells. The test conditions of the accelerated corrosion test are as follows.
Test Conditions of Accelerated Corrosion Test (Stress Corrosion Cracking Resistance Evaluation Test)
Composition of corrosive solution
pH: 3.5-4.5
Processing temperature: 30±10° C.
The reason for adding potassium permanganate as an oxidizer into the corrosive solution is to accelerate the corrosion test.
After the 10-hour test under the above-mentioned test conditions, the samples were taken out from the corrosive solution. Then, the groove portions 1h of the samples were externally examined by use of a magnifier to see if cracking was generated in the groove portions 1h. When the samples were found to be free from cracking, the corrosive solution was replaced with a new one; then, the samples underwent the accelerated corrosion test under the same conditions for another 10 hours. The test was repeated until the cumulative test time reached 80 hours. As a result of the crimping step, a large residual stress is generated in the groove portions 1h. Therefore, by means of the accelerated corrosion test, the groove portions 1h can be evaluated for stress corrosion cracking resistance. In the samples S101 to S103 and S109 to S113, cracking occurred in the groove portions 1h at a cumulative test time of 20 hours or less. In the samples S104, S107, and S108, cracking occurred in the groove portions 1h at a cumulative test time of in excess of 20 hours to less than 50 hours. In the samples S105 and S106, the groove portions 1h were free from cracking even when the cumulative test time reached 80 hours. Thus, the following is understandable: in the case where the Ni strike plating process and the Ni plating process are performed, while the electrolytic chromating process and application of rust prevention oil are not performed, in view of stress corrosion cracking resistance, the Ni plating layer thickness on the inner surface of the metallic shell is preferably 0.3 μm to 2.0 μm, more preferably 0.4 μm to 1.8 μm.
In the second example, metallic shells were manufactured by executing step T100 (Ni strike plating process), step T110 (electrolytic Ni plating process), and step T120 (electrolytic chromating process) of FIG. 3 while omitting step T130 (application of rust prevention oil) of
Processing Conditions of Electrolytic Chromating Process
Processing temperature (bath temperature): 35° C.
Cathode current density: 0.2 A/dm2
Processing time: 5 minutes
Also in the second example, similar to the first example, in order to vary the plating thickness on the inner surface of the groove portion 1h while the plating thickness on the outer surface of the hexagonal portion 1e was held at a fixed value, the processing time of the Ni plating process was varied in a range of 7.5 minutes to 555 minutes, and the cathode current density was varied in a range of 2.4 A/dm2 to 0.032 A/dm2. As a result, the plating thickness on the inner surface of the groove portion 1h was able to be varied in a range of 0.05 μm to 2.5 μm. These samples S201 to S213 were subjected to the above-mentioned test for evaluating stress corrosion cracking resistance.
As shown in
In the third example, metallic shells were manufactured by executing step T100 (Ni strike plating process), step T110 (electrolytic Ni plating process), and step T130 (application of rust prevention oil) of
Also in the third example, similar to the first and second examples, in order to vary the plating thickness on the inner surface of the groove portion 1h while the plating thickness on the outer surface of the hexagonal portion 1e was held at a fixed value, the processing time of the Ni plating process was varied in a range of 7.5 minutes to 555 minutes, and the cathode current density was varied in a range of 2.4 A/dm2 to 0.032 A/dm2. As a result, the plating thickness on the inner surface of the groove portion 1h was able to be varied in a range of 0.05 μm to 2.5 μm. These samples S301 to S313 were subjected to the above-mentioned test for evaluating stress corrosion cracking resistance.
As shown in
In the fourth example, metallic shells were manufactured by executing all of steps T100 to T130 of
Also in the fourth example, similar to the first and third examples, in order to vary the plating thickness on the inner surface of the groove portion 1h while the plating thickness on the outer surface of the hexagonal portion 1e was held at a fixed value, the processing time of the Ni plating process was varied in a range of 7.5 minutes to 555 minutes, and the cathode current density was varied in a range of 2.4 A/dm2 to 0.032 A/dm2. As a result, the plating thickness on the inner surface of the groove portion 1h was able to be varied in a range of 0.05 μm to 2.5 μm. These samples S401 to S413 were subjected to the above-mentioned test for evaluating stress corrosion cracking resistance.
As shown in
In the first to fourth examples mentioned above, the plating thickness of the outer surface of the metallic shell was held at a fixed value of 5 μm; however, in the fifth example, corrosion resistance and plating peeling resistance evaluation tests were conducted for the case where the plating thickness of the outer surface of the metallic shell was varied.
In order to evaluate corrosion resistance, the neutral salt water spray test specified in JIS H8502 was conducted. In this test, after a 48-hour salt spray test, there was measured the percentage of a red-rusted area to the surface area of the metallic shell of a sample. The percentage of a red-rusted area was calculated as follows: a sample after the test was photographed; there were measured a red-rusted area Sa in the photograph and an area Sb of the metallic shell in the photograph; and the ratio Sa/Sb was calculated, thereby obtaining a red-rusted area percentage. The sample S501 exhibited a red-rusted area percentage of in excess of 10%. The samples S502 and S503 exhibited a red-rusted area percentage of in excess of 5% to 10% or less. The sample S504 exhibited a red-rusted area percentage of in excess of 0% to 5% or less. The samples S505 to S509 were free from red rust. In the case where the Ni strike plating process and the Ni plating process are performed, while the electrolytic chromating process and application of rust prevention oil are not performed, in view of salt corrosion resistance, the Ni plating thickness of the outer surface of the metallic shell is preferably 3 μm or more, more preferably 5 μm or more, and most preferably 9 μm or more.
In the plating peeling resistance test, the insulators, etc., were fixed to the metallic shells of the samples by crimping; subsequently, the crimp portions 1d were inspected for a state of plating for evaluation. Specifically, there was measured the percentage of an area where lifting of plating is observed (hereinafter referred to as the “plating lifting area”) to the surface area of the crimp portion 1d. Similar to the measurement of the red-rusted area percentage mentioned above, this measurement was performed by use of photographs. The samples S501 to S506 were free from lifting or peeling of plating, whereas the samples S507 to S509 suffered from lifting or peeling of plating. In the case where the Ni strike plating process and the Ni plating process are performed, while the electrolytic chromating process and application of rust prevention oil are not performed, in view of plating peeling resistance, preferably, the Ni plating thickness of the outer surface of the metallic shell is 15 μm or less.
From the results shown in
In the corrosion resistance test, the sample S601 exhibited a red-rusted area percentage of in excess of 10%. The sample S602 exhibited a red-rusted area percentage of in excess of 5% to 10% or less. The sample S603 exhibited a red-rusted area percentage of in excess of 0% to 5% or less. The samples S604 to S609 were free from red rust. In the case where all of the Ni strike plating process, the Ni plating process, the electrolytic chromating process, and application of rust prevention oil are performed, in view of salt corrosion resistance, the Ni plating thickness of the outer surface of the metallic shell is preferably 3 μm or more, more preferably 4 μm or more, and most preferably 5 μm or more.
In the plating peeling resistance test, the samples S601 to S606 were free from lifting or peeling of plating, whereas the samples S607 to S609 suffered from lifting or peeling of plating. Even in the case where all of the Ni strike plating process, the Ni plating process, the electrolytic chromating process, and application of rust prevention oil are performed, in view of plating peeling resistance, preferably, the Ni plating thickness of the outer surface of the metallic shell is 15 μm or less.
From the results shown in
In the sixth example, the effect of whether or not the Ni strike plating process is provided, on stress corrosion cracking resistance was evaluated.
As shown in
These two groups of samples were subjected to the above-mentioned stress corrosion cracking resistance evaluation test. In this evaluation test, after the elapse of a test time of 24 hours, 100 samples were examined for the number of samples suffering from cracking. In the group of samples having a large Ni plating thickness on the inner surface of the metallic shell, the number of samples suffering from cracking was zero regardless of whether or not the Ni strike plating process was performed. As for the group of samples having a small Ni plating thickness on the inner surface of the metallic shell, in the case where the Ni strike plating process was performed, 80 of 100 samples suffered from cracking, and, in the case where the Ni strike plating process was omitted, 95 of 100 samples suffered from cracking. These test results indicate that the Ni strike plating process somewhat improves stress corrosion cracking resistance. A conceivable reason for improvement of stress corrosion cracking resistance is that the Ni strike plating process fills pinholes in the surface of the metallic shell, thereby improving smoothness of the surface. However, it is understandable that the employment of a sufficiently large Ni plating thickness on the inner surface can ensure sufficient stress corrosion cracking resistance without need to perform the Ni strike plating process.¥
In the seventh example, the effect of the cross-sectional area of the groove portion 1h on stress corrosion cracking resistance was evaluated.
As shown in
These two groups of samples were subjected to the above-mentioned stress corrosion cracking resistance evaluation test. In this evaluation test, after the elapse of a test time of 24 hours, 100 samples were examined for the number of samples suffering from cracking. In the group of samples having a large Ni plating thickness on the inner surface of the metallic shell, the number of samples suffering from cracking was zero regardless of the cross-sectional area of the groove portion 1h. As for the group of samples having a small Ni plating thickness on the inner surface of the metallic shell, cracking occurred in samples in the subgroups having a cross-sectional area of the groove portion 1h of 20 mm2 to 36 mm2. It is understandable from these test results that employment of a large Ni plating thickness on the inner surface of the metallic shell is particularly effective for the metallic shells having a cross-sectional area of the groove portion 1h of 36 mm2 or less.
In the eighth example, the effect of the height of the groove portion 1h on stress corrosion cracking resistance was evaluated.
As shown in
| Number | Date | Country | Kind |
|---|---|---|---|
| 2010-189069 | Aug 2010 | JP | national |
| Filing Document | Filing Date | Country | Kind | 371c Date |
|---|---|---|---|---|
| PCT/JP2011/002158 | 4/12/2011 | WO | 00 | 2/25/2013 |
| Publishing Document | Publishing Date | Country | Kind |
|---|---|---|---|
| WO2012/026049 | 3/1/2012 | WO | A |
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| 6688932 | Nasu et al. | Feb 2004 | B2 |
| 8237341 | Freeman et al. | Aug 2012 | B2 |
| 8421324 | Nasu et al. | Apr 2013 | B2 |
| 8550865 | Uegaki et al. | Oct 2013 | B2 |
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| Number | Date | Country |
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| 2002-184552 | Jun 2002 | JP |
| 2003-257583 | Sep 2003 | JP |
| 2007-23333 | Feb 2007 | JP |
| 2007-141868 | Jun 2007 | JP |
| 2007-270356 | Oct 2007 | JP |
| Entry |
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| Int'l Search Report from corresponding PCT/JP2011/002158 (Form PCT/ISA/210); 1 page. |
| Number | Date | Country | |
|---|---|---|---|
| 20130154468 A1 | Jun 2013 | US |
