CN100458591C - Conductive roll and inspection method therefor - Google Patents
Conductive roll and inspection method therefor Download PDFInfo
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- CN100458591C CN100458591C CNB2005101377862A CN200510137786A CN100458591C CN 100458591 C CN100458591 C CN 100458591C CN B2005101377862 A CNB2005101377862 A CN B2005101377862A CN 200510137786 A CN200510137786 A CN 200510137786A CN 100458591 C CN100458591 C CN 100458591C
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Abstract
The invention provides a conductive roll and an inspection method therefor, stably forming an image and hardly causing a problem such as deletion. This conductive roll includes at least one rubber elastic layer formed of conductive rubber where conductivity is applied to the outer periphery of the core bar by carbon fine powder. In the conductive roll, the relationship between the resistance component Zr([Omega]) and the capacitative reactance component Zc([Omega]) calculated from the impedance ([Omega]) and the phase difference ([theta]) when AC voltage 0.2V with a frequency 1Hz is applied satisfies the expression: Zr/Zc>=5.
Description
Technical field
The present invention relates to employed conductive roll and detection method thereof in the image processing systems such as electrophotographic copier and printer, particularly about developer roll and the method that is applicable to its detection.
Background technology
Employed developer roll in the image processing system uses the material that has added lithium perchlorate plasma conductive agent in polyurethane material.
The shortcoming of having added the developer roll of these ionic conductive agents is that during environmental change, the variation meeting of resistance value is very big.That is, resistance value rises under the low temperature and low humidity environment, the carried charge deficiency of toner, and under hot and humid condition, resistance value diminishes, and toner will be overlapping, and these all are the bad reasons of image.
In addition, the developer roll that provides electric conductivity by carbon black also under study for action, though at this moment smaller to the interdependence of environment, the size that applies voltage can make resistance value, and great changes have taken place.In addition, resistance value has deviation, can't be set at the resistance value of regulation.
Therefore, proposed a kind of developer roll, being provided by carbon black in the developer roll of electric conductivity, can suppress the deviation of resistance value, the resistance value that obtains stipulating can be stablized use (with reference to patent documentation 1).
But,, be to judge actual characteristic when carrying out picture appraisal only by the deviation of resistance value.That is, though the deviation of resistance value equate, evaluation map as the time also can create a difference.
[patent documentation 1]
The spy opens 2003-202750 communique (scope that patent requires etc.)
Summary of the invention
[problem that invention will solve]
The present invention is In view of the foregoing, and purpose is to provide stable conductive roll and the detection method thereof that forms problems such as image, difficult generation blank.
[method of dealing with problems]
The 1st mode of the present invention that addresses the above problem is a kind of conductive roll, the periphery of its axle has the rubber elastic layer that one deck provides the conducting rubber of electric conductivity to constitute by carbon dust at least, it is characterized in that resistive component Zr (Ω) that impedance Z (Ω) when to have applied frequency be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) satisfy following formula (1).
[numerical expression 1]
Zr/Zc≥5 (1)
The 2nd mode of the present invention is a kind of conductive roll, it is characterized in that, in the 1st mode, by applying of under each environment of L/L environment (10 ℃, 30%RH), N/N (25 ℃, 50%RH) and H/H (35 ℃, 85%RH), measuring impedance Z (Ω) and the phase differential θ resistive component Zr (Ω) that calculate and the relation of capacitive reactance component Zc (Ω) of frequency when being the alternating voltage 0.2V of 1Hz satisfy following formula (1).
The 3rd mode of the present invention is a kind of conductive roll, it is characterized in that, in the 1st or the 2nd mode, above-mentioned rubber elastic layer is made of the polyurethane rubber with electric conductivity, and above-mentioned polyurethane is that ether is polyurethane.
The 4th mode of the present invention is a kind of conductive roll, it is characterized in that, in the 3rd mode, be provided with by the surface treatment liquid that comprises isocyanates on the surface of above-mentioned rubber elastic layer and carried out the surface-treated surface-treated layer, resistive component Zr (Ω) that impedance Z (Ω) when to have applied frequency be the alternating voltage 0.2V of 1Hz by the rubber elastic layer after removing this surface-treated layer and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) satisfy following formula (2).
[numerical expression 2]
25≥Zr/Zc≥5 (2)
The 5th mode of the present invention is a kind of conductive roll, it is characterized in that, in the 4th mode, resistive component Zr (Ω) that impedance Z (Ω) when apply frequency to the rubber elastic layer that is provided with above-mentioned surface-treated layer be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) satisfy following formula (2).
The 6th mode of the present invention is a kind of conductive roll, it is characterized in that, in the 4th or the 5th mode, at least a polymkeric substance that above-mentioned surface treatment liquid comprises carbon black or selects from acrylic acid fluorine based polymer, silicon Acrylote based polymer perhaps not only comprises carbon black but also comprise at least a polymkeric substance of selecting from acrylic acid fluorine based polymer, silicon Acrylote based polymer.
The 7th mode of the present invention is a kind of detection method of conductive roll, the axle periphery of this conductive roll has the rubber elastic layer that one deck provides the conducting rubber of electric conductivity to constitute by carbon dust at least, it is characterized in that, detect resistive component Zr (Ω) that impedance Z (Ω) when to have applied frequency be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) and whether satisfy following formula (1).
[numerical expression 3]
Zr/Zc≥5 (1)
The 8th mode of the present invention is a kind of detection method of conductive roll, it is characterized in that, in the 7th mode, whether resistive component Zr (Ω) that impedance Z (Ω) when having detected by applying of mensuration under each environment of L/L environment (10 ℃, 30%RH), N/N (25 ℃, 50%RH) and H/H (35 ℃, 85%RH) frequency and be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) satisfy following formula (1).
The 9th mode of the present invention is a kind of detection method of conductive roll, it is characterized in that, in the 7th or the 8th mode, above-mentioned rubber elastic layer is that the polyurethane rubber that polyurethane rubber constitutes constitutes by the ether with electric conductivity, and be provided with by the surface treatment liquid that comprises isocyanates on the surface of this rubber elastic layer and carried out the surface-treated surface-treated layer, detect resistive component Zr (Ω) that impedance Z (Ω) when to have applied frequency on the rubber elastic layer after removing this surface-treated layer be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) and whether satisfy following formula.
[numerical expression 4]
25≥Zr/Zc≥5 (2)
The 10th mode of the present invention is a kind of detection method of conductive roll, it is characterized in that, in the 9th mode, detect resistive component Zr (Ω) that impedance Z (Ω) when applied frequency to the rubber elastic layer that is provided with above-mentioned surface-treated layer be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) and whether satisfy following formula (2).
The 11st mode of the present invention is a kind of detection method of conductive roll, it is characterized in that, in the 9th or the 10th mode, at least a polymkeric substance that above-mentioned surface treatment liquid comprises carbon black or selects from acrylic acid fluorine based polymer, silicon Acrylote based polymer perhaps not only comprises carbon black but also comprise at least a polymkeric substance of selecting from acrylic acid fluorine based polymer, silicon Acrylote based polymer.
[invention effect]
As described above, according to the present invention, can provide the pass of resistive component Zr (Ω) that impedance Z (Ω) when to have applied frequency be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and capacitive reactance component Zc (Ω) to tie up to conductive roll in the specialized range, reach following effect, characteristic when using as developer roll is highly stable, and is very little to the dependence of environment.
Description of drawings
[Fig. 1] is the microphotograph of conductive roll of observing the state of carbon dispersiveness.
[Fig. 2] is the figure of the frequency characteristic of expression embodiment 1.
[Fig. 3] is the figure of the frequency characteristic of expression comparative example 1.
[Fig. 4] is the figure of the frequency characteristic of expression comparative example 2.
[Fig. 5] is the figure of the frequency characteristic of expression embodiment 5.
[Fig. 6] is the figure of the frequency characteristic of expression comparative example 4.
[Fig. 7] is the figure of the frequency characteristic of expression comparative example 5.
[Fig. 8] is the microphotograph of profile status of the conductive roll of expression embodiment 5.
[Fig. 9] is the microphotograph of profile status of the conductive roll of expression comparative example 4.
[Figure 10] is the microphotograph of profile status of the conductive roll of expression comparative example 5.
[Figure 11] is the frequency characteristic after the grinding again of conductive rollers of expression embodiment 5.
[Figure 12] is the frequency characteristic after the grinding again of conductive rollers of expression comparative example 4.
[Figure 13] is the frequency characteristic after the grinding again of conductive rollers of expression comparative example 5.
[Figure 14] is the figure of the appearance measured of the resistance value of the conductive rollers of expression test example 5.
[Figure 15] is the figure of the frequency characteristic of expression embodiment 11.
[Figure 16] is the figure of the frequency characteristic of expression embodiment 12.
[Figure 17] is the figure of the frequency characteristic of expression comparative example 10.
[Figure 18] is the figure of the frequency characteristic of expression comparative example 11.
[Figure 19] is the microphotograph of profile status of the conductive roll of expression embodiment 11.
[Figure 20] is the microphotograph of profile status of the conductive roll of expression embodiment 12.
[Figure 21] is the microphotograph of profile status of the conductive roll of expression comparative example 10.
[Figure 22] is the microphotograph of profile status of the conductive roll of expression comparative example 11.
[Figure 23] is the frequency characteristic after the grinding again of conductive rollers of expression embodiment 11.
[Figure 24] is the frequency characteristic after the grinding again of conductive rollers of expression embodiment 12.
[Figure 25] is the frequency characteristic after the grinding again of conductive rollers of expression comparative example 10.
[Figure 26] is the frequency characteristic after the grinding again of conductive rollers of expression comparative example 11.
Embodiment
The present invention finishes according to following discovery.In conductive roll with rubber elastic layer that electric conductivity is provided by carbon dust, characteristic such as good picture characteristics is good more more with the disperse state of carbon dust is prerequisite, the actual quality of disperse state can't be judged according to resistance value as in the past, but can be judged by impedance.
Promptly, present inventors find when examining the disperse state of carbon dust, when disperse state is bad a little, can observe the rubber areas that carbon that carbon dust causes in local aggegation comes off, though having or not hardly of the rubber areas that this carbon comes off exerts an influence to resistance value, the resistive component of impedance and phase differential θ and the relation of capacitive reactance component can change.Finish the present invention by above-mentioned discovery.
Conductive roll of the present invention has the conducting rubber elastic layer, in this conducting rubber elastic layer, resistive component Zr (Ω) that impedance Z (Ω) when to have applied frequency be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) satisfy Zr/Zc 〉=5, preferably satisfy the relation of Zr/Zc 〉=10, when having this conducting rubber elastic layer, can be 1 layer of structure, also can be 2 layers of structure.In addition, in order to prevent to pollute and to prevent electric leakage from waiting and when having protective seam and resistive formation, as long as below rubber elastic layer satisfy above-mentioned condition, with regard within the scope of the invention.And, the back can be narrated in detail, rubber elastic layer is made of polyurethane, the surface of this rubber elastic layer is provided with when using the surface treatment liquid that contains isocyanates to carry out the surface-treated surface-treated layer, the rubber elastic layer of removing behind this surface-treated layer need satisfy above-mentioned condition, and for the rubber elastic layer that is provided with surface-treated layer self, resistive component Zr (Ω) that impedance Z (Ω) when to have applied frequency be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) are preferably Zr/Zc 〉=5.
And for example, the carbon that disperses in the way that is shaped aggegation again is bad state, and Zr/Zc can become very big under this state.Present inventors find, when considering that this as a result, are provided with before the surface-treated layer or after surface-treated layer is set and have removed in the rubber elastic layer of this surface-treated layer, preferably satisfy 25 〉=Zr/Zc.That is, do not satisfy the condition of 25 〉=Zr/Zc and satisfy after being provided with surface-treated layer in the rubber elastic layer of condition of 25 〉=Zr/Zc before surface-treated layer is set, carbon may carry out aggegation again, and this is improper.Certainly, it is also improper all can not to satisfy the rubber elastic layer of 25 〉=Zr/Zc condition in the front and back that surface-treated layer is set.
Here, the cross sectional photograph of the rubber elastic layer of the conductive roll of carbon particulate formation as shown in Figure 1.(a) being the good situation of disperse state, (b) is the bad situation of disperse state, and (b) middle black part is divided into the rubber areas that carbon particulate comes off.The equivalent electrical circuit of such rubber elastic layer can be by the resistive component of the carbon tissue that forms conductive path and the heat when being shaped and disperse bad etc. to cause aggegation, the parallel circuit of capacitive reactance component that do not form the carbon tissue of conductive path represents, when the rubber areas that disperse state worsens, carbon comes off becomes big, because forming the carbon tissue of conductive path tails off, on the contrary, the carbon tissue that does not form conductive path becomes many, so resistive component reduces and capacitive reactance component Zc rises, and can not keep the relation of Zr/Zc 〉=5.
When making the conductive roll of the invention described above, as long as it is just passable to improve the dispersiveness of carbon particulate as far as possible, its manufacture method is not particularly limited, but when adopting following manufacture method, can make good dispersion easily and have the rubber elastic layer of the impedance of satisfying above-mentioned relation.Certainly, because how many this methods has deviation, so can not guarantee to be met the rubber elastic layer of above-mentioned relation.
Finished detection method of the present invention according to above-mentioned viewpoint.Promptly, detection method of the present invention is, in the detection method of conductive roll, detect resistive component Zr (Ω) that impedance Z (Ω) when to have applied frequency be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) and whether satisfy following formula (1).In addition, for the rubber elastic layer of removing after the rubber elastic layer before the surface-treated layer being set or being provided with surface-treated layer, detect resistive component Zr (Ω) that impedance Z (Ω) when to have applied frequency be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) and whether satisfy following formula (2).
Thus, reach following effect, for example, just can judge without the detected image characteristic and the quality of the dispersiveness of carbon particulate can significantly reduce the defective of end article.
[numerical expression 5]
Zr/Zc≥5 (1)
[numerical expression 6]
25≥Zr/Zc≥5 (2)
The manufacture method of dispersed carbon particulate is preferably, carbon dust is dispersed in the manufacture method that the conductive elastic layer that constitutes in the thermo-setting elastomer is formed on the conductive roll on the axle, it is characterized in that, on the forming face of the shaping dies that forms above-mentioned conductive elastic layer, low 1 figure place of this shaping dies of thermal conductivity ratio or the above low heat conductivity pipe of 1 figure place are set, preferably replace shaping dies, the low heat conductivity pipe as moulding material, is placed in electrothermal furnace etc. and adds the above-mentioned conductive elastic layer of thermosetting.Here, the low heat conductivity pipe is preferably resin pipe, and the thickness of low heat conductivity pipe is preferably 0.05～1.00mm, and the pyroconductivity of low heat conductivity pipe is preferably 0.1W/mK～5W/mK.
But, the manufacture method of conductive roll of the present invention is not limited thereto, even common mold heated is shaped, as long as can guarantee that the dispersiveness of carbon particulate is just passable, for example, can trickle control mold temperature react,, appear at the surface until the position of the good dispersion of carbon particulate perhaps to utilizing rapid thermal gradient to scrape deeply at the conductive elastic laminar surface that near surface has carried out the conductive roll of carbon aggegation.
In addition, detection method of the present invention can be applicable to the conductive roll made from any manufacture method, when the dispersiveness that is used for carbon particulate is easy to generate the conductive roll that the manufacture method of deviation makes, can significantly reduce disqualification rate.
In the conductive roll of the present invention, carbon particulate is, based at least a carbon black of conductive carbon black etc., certainly, also multiple carbon black can be mixed and use, at this moment, generally based on conductive carbon black.
And the addition of carbon black is different and different according to the resistance value of target, for example, when adding ether to and being polyurethane, is polyvalent alcohol for the ether of 100 weight portions, preferably is less than or equal to 8 weight portions.When surpassing 8 weight portions, be difficult to be shaped.
In addition, the elastomeric material that constitutes rubber elastomer of the present invention can be selected according to use, is not particularly limited, but considers that photoreceptor pollutes and rubber property during the developing roller, and being preferably polyurethane, particularly ether is polyurethane.In addition, during for polyurethane, has following advantage: the surface-treated layer after being handled by the surface treatment liquid that contains isocyanates can be set.
Conductive roll of the present invention, protective seam and resistive formation can be the structures of the pipe of covering resin system etc., and the surface-treated layer after carrying out surface treatment by the surface treatment liquid that contains isocyanates also can be set on the elastic layer surface.This is because compare when having covered coated tube, and the resistance value of the surface-treated layer that said method forms can great changes will take place, and all well and good on the non-polluting this point yet.Promptly, after above-mentioned surface-treated layer is set, the tissue of the carbon black in the zone, top layer of formation surface-treated layer is cut off from the surface to the inside gradually, the inclination resistive layer of the inclination that the formation resistance value diminishes gradually, addition and inclination resistive layer by carbon black suitably is set can access desired resistance value.
In addition, conductive roll of the present invention is preferably provided electric conductivity and is not contained ionic conductive agent by carbon dust.Because the environment interdependence of resistance value just becomes minimum like this.And the resistance value of conductive roll changes along with applying voltage, but apply 5V respectively, the resistance value Rv when 50V, 100V
5, Rv
50, Rv
100Be preferably in 5 * 10
5～5 * 10
8In the scope of Ω.
The ether that is fit to the base material of rubber elastomer of the present invention is polyurethane, can obtain promptly so-called injection type polyurethane by the polyvalent alcohol and the polyisocyanate reaction that based on ether are polyvalent alcohol.This is in order to reduce compressive strain.And, even ether is polyurethane, compressive strain can not be fallen very low during for Miller Pu Lip river type.In addition, when using ester class polyurethane, it is bad to add the water decomposition characteristic, can not steady in a long-termly use.
The compressive strain of the rubber elastic layer of conductive roll of the present invention (JIS K6262) is preferably smaller or equal to 3%.This is that carried charge can produce deviation because greater than 3% o'clock.
Diisocyanate with the PTMEG reaction, for example, 2,4-toluene diisocyanate (TDI), 4,4 '-methyl diphenylene diisocyanate (MDI), PPDI (PPDI), 1,5-naphthalene diisocyanate (NDI), 3,3-dimethyl hexichol-4,4 '-diisocyanate (TODI) and two ends have these the modification body of prepolymer etc. of isocyanates and polymkeric substance etc.
In addition, elastomeric top layer part must be handled and carried out surface treatment by the above-mentioned isocyanates that hardens in the isocyanate compound that is immersed in.Surface treatment liquid used herein is that isocyanate compound is dissolved in the organic solvent, can also add carbon black.In addition, can also use in the organic solvent that has dissolved isocyanate compound, add the material of at least a polymkeric substance of from acrylic acid fluorine based polymer and silicon Acrylote based polymer, selecting, but also can use materials such as having added above-mentioned polymkeric substance and conductivity additive.
Here, isocyanate compound for example, 2,6-toluene diisocyanate (TDI), 4,4 '-methyl diphenylene diisocyanate (MDI), PPDI (PPDI), 1,5-naphthalene diisocyanate (NDI), 3,3-dimethyl hexichol-4,4 '-diisocyanate (TODI) and above-mentioned polymkeric substance and modification body etc.
And conductive roll of the present invention is specially adapted to developer roll, and in order to use as developer roll is stable, the surfaceness Rz that circumferencial direction is measured is preferably smaller or equal to 8 μ m.
According to embodiment the present invention is described below, but the present invention is not limited thereto.
[embodiment]
(embodiment 1)
(method for making of roller) is the GP-3000 (ProductName of polyvalent alcohol 100 weight portions as polyethers, Sanyo changes into company and makes) the middle black #5500 (ProductName of ト one カ that adds 5 weight portions, East Sea carbon company makes), discrete particles, make it smaller or equal to 10 μ m, with adjustment is 60 ℃, obtains A liquid.In addition, in the prepolymer ア of 25 weight portions ジ プ レ Application L100 (ProductName, ユ ニ ロ イ ヤ Le company make), add the コ ロ ネ one ト C-HX that mixes 11 weight portions (ProductName, Japanese polyurethane company makes),, obtain B liquid adjustment to 60 ℃.Mix this A liquid and B liquid, inject by polypropylene system resin pipe box the two ends of axle are fixed in advance in case with axle (
L:270mm) be arranged in the polypropylene system ejector sleeve (external diameter 24mm, thick 0.3mm) of central authorities, heating is 120 minutes in 110 ℃ baker, removes two ends, obtains the roller that the axle surface forms the electric conductivity polyurethane layer.The concentration of carbon black is 3.5wt%.
With the surface grinding 1.5mm of this conductive roll, conductive roll that external diameter is adjusted into 20mm conductive roll as embodiment 1.
(embodiment 2)
Except the thickness of polypropylene system ejector sleeve was 0.2mm, other and embodiment 1 the same manufacturing were as the conductive roll of embodiment 2.
(embodiment 3)
Except heating-up temperature was 130 ℃, other and embodiment 1 the same manufacturing were as the conductive roll of embodiment 3.
(embodiment 4)
Except heating-up temperature was 130 ℃, other and embodiment 2 the same manufacturings were as the conductive roll of embodiment 4.
(embodiment 5)
Use surface treatment liquid that the conductive roll of embodiment 1 is carried out surface treatment, form surface-treated layer.This surface treatment liquid is with the ethyl acetate of 100 weight portions, the acetylene black of 3 weight portions (manufacturing of electrochemical company) and 2 parts by weight of acrylic fluorine based polymer (ノ バ fluorine: (ProductName) by bowl mill, the true qualities material was made in big day) dispersing and mixing is after 3 hours, and interpolation mixes isocyanate compound (MDI) the back dissolving of 20 weight portions and forms.That is, surface treatment liquid is remained on 23 ℃, rubber rollers was soaked for 10 seconds, in 120 ℃ baking oven, heated 1 hour then, form surface-treated layer, as the conductive roll of embodiment 5.
(embodiment 6)
The processing the same with embodiment 5 carried out on the surface of the conductive roll of embodiment 2, as the conductive roll of embodiment 6.
(embodiment 7)
The processing the same with embodiment 5 carried out on the surface of the conductive roll of embodiment 3, as the conductive roll of embodiment 7.
(embodiment 8)
The processing the same with embodiment 5 carried out on the surface of the conductive roll of embodiment 4, as the conductive roll of embodiment 8.
(comparative example 1)
Except smear as release layer silicon be release agent and be injected in the iron pipe mould that is preheating to 110 ℃, other and embodiment 1 the same manufacturing are adjusted to 20mm with the top layer attrition process into about the thickness of 1.5mm and with external diameter, as a comparative example 1 conductive roll.
(comparative example 2)
Make it tight contact of inwall with the iron pipe mould other and comparative example 1 the same manufacturing, 2 conductive roll as a comparative example except inserting polypropylene system ejector sleeve (external diameter 23mm, thickness 0.3mm).
(comparative example 3)
Except heating-up temperature is 130 ℃, other and comparative example 1 the same manufacturing, 3 conductive roll as a comparative example.
(comparative example 4)
The processing the same with embodiment 5,4 conductive roll are as a comparative example carried out in the surface of the conductive roll of comparative example 1.
(comparative example 5)
The processing the same with embodiment 5,5 conductive roll are as a comparative example carried out in the surface of the conductive roll of comparative example 2.
(comparative example 6)
The processing the same with embodiment 5,6 conductive roll are as a comparative example carried out in the surface of the conductive roll of comparative example 3.
(comparative example 7)
Except conductive agent adds the lithium perchlorate of 0.1 weight portion,, carry out the processing the same simultaneously, as a comparative example 7 conductive roll with embodiment 5 with comparative example 1 the same manufacturing.
(test example 1)＜impedance measuring 〉
(BHA company makes to use the impedance analysis device; Impedance analysis device IM6e) impedance operator of each conductive roll of mensuration embodiment and comparative example (except comparative example 7).During mensuration, under the state of N/N environment (25 ℃, 50%RH), the additional 500g load in roller two ends, applying voltage is that 0.2V measures, and impedance Z when being 1Hz by a-c cycle (Ω) and phase differential θ calculate the ratio Zr/Zc of resistive component Zr (Ω) and capacitive reactance component Zc (Ω).
The result of embodiment 1～4 and comparative example 1～3 is as shown in table 1, and the result who has formed the embodiment 5～8 of surface-treated layer and comparative example 4～6 is as shown in table 2.In addition, the frequency characteristic of embodiment 1 and comparative example 1,2, embodiment 5 and comparative example 4,5 such as Fig. 2～shown in Figure 7.
(test example 2)＜picture appraisal 〉
The developer roll of embodiment 5～8 and comparative example 4～7 is installed in the printer of selling on the market, under L/L environment (10 ℃, 30%RH), N/N (25 ℃, 50%RH) and H/H (35 ℃, 85%RH), carries out picture appraisal respectively.Its result is illustrated in the table 2 in the lump.
The microscopic examination of (test example 3)＜roller section 〉
(KEYENCE company makes with laser microscope; VK-9500) section of the developer roll of observation embodiment and comparative example, the deployment conditions of evaluation carbon.Its result is as shown in table 2.In addition, the microphotograph of embodiment 5 and comparative example 4,5 such as Fig. 8～shown in Figure 10.
[table 1]
| Embodiment 1 | |
Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Zr/Zc | 5.25 | 5.17 | 5.17 | 5.59 | 1.61 | 2.43 | 2.13 |
[table 2]
| Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Comparative example 4 | Comparative example 5 | Comparative example 6 | Comparative example 7 | |
| Zr/Zc | 5.98 | 6.78 | 5.59 | 8.40 | 2.10 | 4.08 | 2.36 | - |
| Picture appraisal L/L | Well | Well | Well | Well | Lettering concentration has deviation | Common | Lettering concentration has deviation | The lettering deficiency |
| Picture appraisal N/N | Well | Well | Well | Well | Lettering concentration has deviation | Common | Lettering concentration has deviation | Well |
| Picture appraisal H/H | Well | Well | Well | Well | Lettering concentration has deviation | Common | Lettering concentration has deviation | Overlap |
| Carbon disperses | Well | Well | Well | Well | Defective | Disperse inhomogeneous | Defective | - |
(test example 4)＜again impedance measuring of grinding object 〉
Developing roller surface to embodiment 5～8 and comparative example 4～6 is ground 0.5mm again, removes surface-treated layer, equally with test example 1 measures impedance, obtains Zr/Zc.Its result is as shown in table 3.In addition, the frequency characteristic of embodiment 5 and comparative example 4,5 such as Figure 11～shown in Figure 13.
[table 3]
| Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| Zr/Zc | 5.80 | 5.59 | 5.13 | 5.27 | 4.23 | 4.50 | 4.39 |
(test example 5)
Deviation to resistance value is estimated.That is, as shown in figure 14, be the stainless steel electrode 51 of 2mm the wide of surface adhesion electrode of the rubber elastic layer 12 of conductive roll, the roller that limit rotation and axle are 11, its locational resistance value is measured on the limit.6 local mensuration of length direction, obtain the maximal value R of mean value
MaxAnd minimum value R
MinIts result is as shown in table 4.
[table 4]
| R max | R min | R max/R min | |
| Embodiment 1 | 2.19×10 6 | 1.08×10 6 | 2 |
| |
1.79×10 6 | 7.82×10 5 | 2 |
| Embodiment 3 | 1.77×10 6 | 7.51×10 5 | 2 |
| Embodiment 4 | 1.79×10 6 | 7.61×10 5 | 2 |
| Embodiment 5 | 1.06×10 7 | 4.35×10 6 | 2 |
| Embodiment 6 | 1.45×10 7 | 4.24×10 6 | 3 |
| Embodiment 7 | 4.87×10 6 | 2.06×10 6 | 2 |
| Embodiment 8 | 8.01×10 6 | 2.37×10 6 | 3 |
| Comparative example 1 | 2.27×10 6 | 9.28×10 5 | 2 |
| Comparative example 2 | 1.71×10 6 | 7.18×10 5 | 2 |
| Comparative example 3 | 2.16×10 6 | 8.72×10 5 | 2 |
| Comparative example 4 | 6.14×10 7 | 6.60×10 6 | 9 |
| Comparative example 5 | 3.11×10 7 | 4.97×10 6 | 6 |
| Comparative example 6 | 1.71×10 7 | 2.02×10 6 | 8 |
(embodiment 9)
Carbon dust uses the VULCUN XC (ProductName, キ ヤ ボ Star ト company makes) of black #5500 of ト one カ of 4 weight portions (ProductName, carbon company in the East Sea makes) and 3 weight portions, discrete particles, make it smaller or equal to 20 μ m, other and embodiment 1 the same manufacturing are as the conductive roll of embodiment 9.
(embodiment 10)
Replace polypropylene system ejector sleeve, using and having smeared silicon is release agent, and is injected into the iron pipe mould that is preheating to 90 ℃, and other and embodiment 9 the same manufacturings are as the conductive roll of embodiment 10.
(embodiment 11)
The processing the same with embodiment 5 carried out on the surface of the conductive roll of embodiment 9, as the conductive roll of embodiment 11.
(embodiment 12)
The processing the same with embodiment 5 carried out on the surface of the conductive roll of embodiment 10, as the conductive roll of embodiment 12.
(comparative example 8)
For carbon dust, add the BYK-9076 as spreading agent (ProductName, PVC Star Network ケ ミ one Japan company makes) of 30 weight %, discrete particles makes it smaller or equal to 10 μ m, other and embodiment 9 the same manufacturing, 8 conductive rolls as a comparative example.
(comparative example 9)
Except heating-up temperature is 90 ℃, other and embodiment 9 the same manufacturing, 9 conductive rolls as a comparative example.
(comparative example 10)
The processing the same with embodiment 5,10 conductive roll are as a comparative example carried out in the surface of the conductive roll of comparative example 8.
(comparative example 11)
The processing the same with embodiment 5,11 conductive roll are as a comparative example carried out in the surface of the conductive roll of comparative example 9.
(test example 6)＜impedance measuring 〉
(BHA company makes to use the impedance analysis device; Impedance analysis device IM6e) impedance operator of each conductive roll of mensuration embodiment 9～12 and comparative example 8～11.During mensuration, under the state of N/N environment (25 ℃, 50%RH), the additional 500g load in roller two ends, applying voltage is that 0.2V measures, resistive component Zr (Ω) that impedance Z when being 1Hz by a-c cycle (Ω) and phase differential θ calculate and the ratio Zr/Zc of capacitive reactance component Zc (Ω).
The result of embodiment 9～10 and comparative example 8～9 is as shown in table 5, and the result who has formed the embodiment 11～12 of surface-treated layer and comparative example 10～11 is as shown in table 6.In addition, the frequency characteristic of embodiment 11 and 12, comparative example 10,11 such as Figure 15～shown in Figure 180.
(test example 7)＜picture appraisal 〉
The developer roll of embodiment 11～12 and comparative example 10～11 is installed in the printer of selling on the market, under L/L environment (10 ℃, 30%RH), N/N (25 ℃, 50%RH) and H/H (35 ℃, 85%RH), carries out picture appraisal respectively.Its result is illustrated in the table 6 in the lump.
The microscopic examination of (test example 8)＜roller section 〉
(KEYENCE company makes with microscope; VHX-100) section of the developer roll of observation embodiment 11～12 and comparative example 10～11, the deployment conditions of evaluation carbon.Its result is illustrated in the table 6 in the lump.In addition, the microphotograph of embodiment 11～12 and comparative example 10～11 such as Figure 19～shown in Figure 22.
[table 5]
| Embodiment 9 | Embodiment 10 | Comparative example 8 | Comparative example 9 | |
| Zr/Zc | 16.21 | 12.03 | 3.66 | 28.49 |
[table 6]
| |
|
Comparative example 10 | Comparative example 11 | |
| Zr/Zc | 8.24 | 7.78 | 2.30 | 8.76 |
| Picture appraisal L/L | Well | Well | Lettering concentration has deviation | Common |
| Picture appraisal N/N | Well | Well | Lettering concentration has deviation | Common |
| Picture appraisal H/H | Well | Well | Lettering concentration has deviation | Common |
| Carbon disperses | Well | Well | Very good | Disperse inhomogeneous |
(test example 9)＜again impedance measuring of grinding object 〉
The developing roller surface of embodiment 11～12 and comparative example 10～11 is ground 0.5mm again, remove surface-treated layer, equally with test example 6 measure impedance, obtain Zr/Zc.Its result is as shown in table 7.In addition, the frequency characteristic of embodiment 11～12 and comparative example 10～11 such as Figure 23～shown in Figure 26.
[table 7]
| |
|
Comparative example 10 | Comparative example 11 | |
| Zr/Zc | 13.58 | 10.84 | 1.61 | 28.78 |
(test example 10)
Deviation to resistance value is estimated.That is, as shown in figure 14, be the stainless steel electrode 51 of 2mm the wide of surface adhesion electrode of the rubber elastic layer 12 of conductive roll, the roller that limit rotation and axle are 11, its locational resistance value is measured on the limit.6 local mensuration of length direction, obtain the maximal value R of mean value
MaxAnd minimum value R
MinIts result is as shown in table 8.
[table 8]
| R max | R min | R max/R min | |
| Embodiment 9 | 7.10×10 6 | 4.29×10 6 | 2 |
| Embodiment 10 | 8.11×10 6 | 4.18×10 6 | 2 |
| |
5.26×10 6 | 9.83×10 5 | 5 |
| |
7.21×10 6 | 1.45×10 6 | 5 |
| Comparative example 8 | 1.55×10 9 | 1.00×10 7 | 155 |
| Comparative example 9 | 7.05×10 5 | 3.11×10 5 | 2 |
| Comparative example 10 | 3.65×10 9 | 2.08×10 8 | 18 |
| Comparative example 11 | 5.09×10 6 | 9.10×10 5 | 6 |
(test findings)
By above-mentioned test findings, can learn to draw a conclusion.
Result according to test example 1, in the conductive roll by the embodiment 1～4 of the dispersiveness manufacture method manufacturing preferably of carbon dust, resistive component Zr (Ω) that is calculated by impedance Z (Ω) and phase differential θ and the ratio Zr/Zc of capacitive reactance component Zc (Ω) are more than or equal to 5, and in the conductive roll of the comparative example 1～4 that is produced by the dispersed not so good manufacture method of carbon dust, Zr/Zc is less than 5.
In addition, according to the result of test example 2～4, the conductive roll of embodiment 1～4 has been carried out in the conductive roll of surface-treated embodiment 5～8, Zr/Zc is more than or equal to 5, but the conductive roll to comparative example 1～3 has carried out in the conductive roll of surface-treated comparative example 4～6, and Zr/Zc is littler than 5.
In addition, the result that portrait is estimated confirms, when using Zr/Zc greater than the conductive roll of 5 embodiment 5～8, the image in each environment is good, and is also good with the observed carbon dispersiveness of microphotograph.And in the conductive roll of Zr/Zc less than 5 comparative example 4～6, picture appraisal is bad, and in addition, carbon disperses also inhomogeneous.And the conductive roll that has added the comparative example 7 of ionic conductive agent also has problem in picture appraisal.
And, the Zr/Zc that the conductive roll that has carried out surface-treated embodiment 5～8 is measured, in milled processed, remove surface-treated layer after, bigger than 5.
In addition, the generation of the deviation of the resistance value that the conductive roll of embodiment 1～8 and comparative example 1～6 is measured, irrelevant with the quality of carbon dispersiveness.Thus, carbon favorable dispersibility and portrait characteristic good electrical conductivity roller can not be judged fully with the deviation of resistance value, but can estimate with Zr/Zc.
In addition, among the embodiment 9, increase the amount of carbon, and make particle smaller or equal to 20 μ m, dispersiveness is lower than embodiment 1～4 and is shaped, but owing to be to make with the manufacture method of the favorable dispersibility of carbon dust, so Zr/Zc is more than or equal to 5, resistive component is not only all big than embodiment 1～4, and more than or equal to 10.
Embodiment 10 makes with the dispersed bad manufacture method of carbon dust, but may be because forming temperature drops to 90 ℃ cause, and near the aggegation of the carbon the die surface is suppressed, and Zr/Zc is more than or equal to 5.
On the contrary, the comparative example 8 that use spreading agent, carbon is disperseed more has only dispersed very good, and because the cause that can not be completed into by the conductive path of carbon organizational composition, Zr/Zc is less than 5.In addition, in the comparative example 9, forming temperature drops to 90 ℃, though produced by the manufacture method of the favorable dispersibility of carbon dust, may be because the sclerous reaction of poly-imines fat is too slow, and carbon has carried out aggegation again, makes Zr/Zc than 25 also greatly.
Here, the result of picture appraisal confirms, when using Zr/Zc greater than the conductive roll of 5 embodiment 11,12, the image in each environment is good, and the observed carbon dispersiveness of microphotograph is also good.And in the conductive roll of Zr/Zc, observe to such an extent that the carbon dispersiveness is very good by microphotograph, but in the picture appraisal, lettering concentration have deviation less than 5 comparative example 10.
And in the Zr/Zc of the rubber elastic layer conductive roll greater than 25 comparative example 11, the image in each environment is general, but from the observed carbon dispersiveness of microphotograph, by the aggegation again of carbon caused disperse inhomogeneous.
And, the Zr/Zc that the conductive roll that has carried out surface-treated embodiment 11,12 is measured, in milled processed, remove surface-treated layer after, bigger than 5.
In addition, the quality of the generation of the deviation of the resistance value that the conductive roll of embodiment 9～12 and comparative example 8～11 is measured and carbon dispersiveness is irrelevant.Thus, carbon favorable dispersibility and portrait characteristic good electrical conductivity roller can not be judged fully with the deviation of resistance value, but can estimate with Zr/Zc.
Claims (11)
1. conductive roll, the periphery of its axle has the rubber elastic layer that one deck provides the conducting rubber of electric conductivity to constitute by carbon dust at least, it is characterized in that, resistive component Zr (Ω) that impedance Z (Ω) when to have applied frequency be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) satisfy following formula (1)
[numerical expression 1]
Zr/Zc≥5(1)。
2. conductive roll as claimed in claim 1, it is characterized in that, by applying of under each environment of 10 ℃ and 30%RH, 25 ℃ and 50%RH and 35 ℃ and 85%RH, measuring impedance Z (Ω) and the phase differential θ resistive component Zr (Ω) that calculate and the relation of capacitive reactance component Zc (Ω) of frequency when being the alternating voltage 0.2V of 1Hz satisfy following formula (1).
3. conductive roll as claimed in claim 1 or 2 is characterized in that, above-mentioned rubber elastic layer is made of the polyurethane rubber with electric conductivity, and above-mentioned polyurethane is that ether is polyurethane.
4. conductive roll as claimed in claim 3, it is characterized in that, be provided with on the surface of above-mentioned rubber elastic layer with the surface treatment liquid that comprises isocyanates and carried out the surface-treated surface-treated layer, resistive component Zr (Ω) that impedance Z (Ω) when to have applied frequency be the alternating voltage 0.2V of 1Hz by the rubber elastic layer after removing this surface-treated layer and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) satisfy following formula (2)
[numerical expression 2]
25≥Zr/Zc≥5(2)。
5. conductive roll as claimed in claim 4, it is characterized in that resistive component Zr (Ω) that impedance Z (Ω) when apply frequency to the rubber elastic layer that is provided with above-mentioned surface-treated layer be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) satisfy following formula (2).
6. conductive roll as claimed in claim 5, it is characterized in that, at least a polymkeric substance that above-mentioned surface treatment liquid comprises carbon black or selects from acrylic acid fluorine based polymer and silicon Acrylote based polymer perhaps not only comprises carbon black but also comprise at least a polymkeric substance of selecting from acrylic acid fluorine based polymer and silicon Acrylote based polymer.
7. the detection method of a conductive roll, the axle periphery of this conductive roll has the rubber elastic layer that one deck provides the conducting rubber of electric conductivity to constitute by carbon dust at least, it is characterized in that, whether impedance Z (Ω) and the phase differential θ resistive component Zr (Ω) that calculate and the relation of capacitive reactance component Zc (Ω) of detection when to have applied frequency be the alternating voltage 0.2V of 1Hz satisfies following formula (1)
[numerical expression 3]
Zr/Zc≥5(1)。
8. the detection method of conductive roll as claimed in claim 7, it is characterized in that whether resistive component Zr (Ω) that impedance Z (Ω) when having detected by applying of measuring frequency and be the alternating voltage 0.2V of 1Hz under each environment of 10 ℃ and 30%RH, 25 ℃ and 50%RH and 35 ℃ and 85%RH and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) satisfy following formula (1).
9. as the detection method of claim 7 or 8 described conductive rolls, it is characterized in that, above-mentioned rubber elastic layer is that the polyurethane rubber that polyurethane rubber constitutes constitutes by the ether with electric conductivity, and be provided with on the surface of this rubber elastic layer with the surface treatment liquid that comprises isocyanates and carried out the surface-treated surface-treated layer, detect resistive component Zr (Ω) that impedance Z (Ω) when to have applied frequency on the rubber elastic layer after removing this surface-treated layer be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) and whether satisfy following formula (2).
[numerical expression 4]
25≥Zr/Zc≥5(2)
10. the detection method of conductive roll as claimed in claim 9, it is characterized in that, detect resistive component Zr (Ω) that impedance Z (Ω) when applied frequency to the rubber elastic layer that is provided with above-mentioned surface-treated layer be the alternating voltage 0.2V of 1Hz and phase differential θ calculate and the relation of capacitive reactance component Zc (Ω) and whether satisfy following formula (2).
11. the detection method of conductive roll as claimed in claim 10, it is characterized in that, at least a polymkeric substance that above-mentioned surface treatment liquid comprises carbon black or selects from acrylic acid fluorine based polymer and silicon Acrylote based polymer perhaps not only comprises carbon black but also comprise at least a polymkeric substance of selecting from acrylic acid fluorine based polymer and silicon Acrylote based polymer.
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| JP2004279731A (en) * | 2003-03-14 | 2004-10-07 | Hokushin Ind Inc | Electrifying roll |
| CN1680883A (en) * | 2004-04-08 | 2005-10-12 | 北辰工业株式会社 | Conductive roll and method for producing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004279731A (en) * | 2003-03-14 | 2004-10-07 | Hokushin Ind Inc | Electrifying roll |
| CN1680883A (en) * | 2004-04-08 | 2005-10-12 | 北辰工业株式会社 | Conductive roll and method for producing same |
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