US 12,730,390 B2Granted

Fine particle, external additive for toners, and toner

AssigneeCanon Kabushiki Kaisha

InventorsIchiro Kanno, Hiroki Watanabe, Mari Kaburagi, Hayato Ida

Life of this patent

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Abstract

The fine particle is a silicon-containing fine particle, wherein the number-average diameter of the fine particle is 0.05 μm to 0.30 μm; the proportion of the silicon atom with reference to the total of the elements is at least 20% according to fluorescent x-ray measurement of the fine particle; and, with respect to the silicon atom proportions measured in analysis by x-ray photoelectron spectroscopy while irradiating with Ar-Kα radiation and etching, the proportions of silicon atoms having prescribed structures vary at prescribed depths.

Claims9

Dependent claims

A fine particle, comprising:

silicon;
the fine particle having a number-average primary particle diameter of 0.05 to 0.30 μm;
the proportion of a silicon atom with reference to a total of elements being at least 20% according to fluorescent x-ray measurement of the fine particle;
and
with respect to the silicon atom proportions measured in analysis by x-ray photoelectron spectroscopy while irradiating with Ar-Kα radiation and etching, and using a total detected silicon atom peak area for total peak area of the silicon atom at a binding energy of 102.0 to 104.0 eV,
when X is a proportion (atomic %) in the total detected silicon atom peak area of a peak area at a binding energy of 103.5 to 104.0 eV that corresponds to silicon atoms having a structure given by following (a), and Y is a sum of proportions (atomic %) in the total detected silicon atom peak area of peak areas at a binding energy of 102.0 to 103.4 eV that correspond to silicon atoms having structures given by following formula formulae (b), (c) and (d)
where R1, R2, R3, R4, R5 and R6 independently represent an alkyl group or a phenyl group
(i) Y<X is constantly satisfied in Condition A measurement range, and
(ii) a point of transition from Y<X to Y>X is present in Condition B measurement range and Y>X is constantly satisfied after the transition
Condition A:
for a polyethylene terephthalate test specimen, time for which a starting point is time required to erode a depth of 2 nm by irradiation with Ar-Kα radiation and for which an end point is time required to erode a depth of 10 nm, and
Condition B:
for a polyethylene terephthalate test specimen, time for which a starting point is time required to erode a depth of 10 nm by irradiation with Ar-Kα radiation and for which an end point is time required to erode a depth of 20 nm, wherein
0.30≤S4/SA≤0.80
0.00≤S3/SA≤0.50
0.20≤S2/SA≤0.70
when in a chart obtained by 29Si-NMR measurement of the fine particle, SA is a total peak area corresponding to silicon polymer, S4 is a peak area corresponding to formula (a), S3 is a peak area corresponding to formula (b), and S2 is a peak area corresponding to formula (c) where R1, R2 and R3 independently represent an alkyl group having 1 to 6 carbons.

14 more elements

An external additive for toner, comprising:

a fine particle comprising silicon;
the fine particle having a number-average primary particle diameter of 0.05 to 0.30 μm;
the proportion of a silicon atom with reference to a total of elements being at least 20% according to fluorescent x-ray measurement of the fine particle;
and
with respect to the silicon atom proportions measured in analysis by x-ray photoelectron spectroscopy while irradiating with Ar-Kα radiation and etching, and using a total detected silicon atom peak area for total peak area of the silicon atom at a binding energy of 102.0 to 104.0 eV,
when X is a proportion (atomic %) in the total detected silicon atom peak area of a peak area at a binding energy of 103.5 to 104.0 eV that corresponds to silicon atoms having a structure given by following (a), and Y is a sum of proportions (atomic %) in the total detected silicon atom peak area of peak areas at a binding energy of 102.0 to 103.4 eV that correspond to silicon atoms having structures given by following formula formulae (b), (c) and (d)
where R1, R2, R3, R4, R5 and R6 independently represent an alkyl group or a phenyl group
(i) Y<X is constantly satisfied in Condition A measurement range described below, and
(ii) a point of transition from Y<X to Y>X is present in Condition B measurement range and Y>X is constantly satisfied after the transition
Condition A:
for a polyethylene terephthalate test specimen, time for which a starting point is time required to erode a depth of 2 nm by irradiation with Ar-Kα radiation and for which an end point is time required to erode a depth of 10 nm, and
Condition B:
for a polyethylene terephthalate test specimen, time for which a starting point is time required to erode a depth of 10 nm by irradiation with Ar-Kα radiation and for which an end point is time required to erode a depth of 20 nm.,
wherein
0.30≤S4/SA≤0.80
0.00≤S3/SA≤0.50
0.20≤S2/SA≤0.70
when in a chart obtained by 29Si-NMR measurement of the fine particle, SA is a total peak area corresponding to silicon polymer, S4 is a peak area corresponding to formula (a), S3 is a peak area corresponding to formula (b), and S2 is a peak area corresponding to formula (c) where R1, R2 and R3 independently represent an alkyl group having 1 to 6 carbons.

15 more elements

A toner, comprising:

a toner particle;
and
a fine particle comprising silicon;
the fine particle having a number-average primary particle diameter of 0.05 to 0.30 μm;
the proportion of a silicon atom with reference to a total of elements being at least 20% according to fluorescent x-ray measurement of the fine particle;
and
with respect to the silicon atom proportions measured in analysis by x-ray photoelectron spectroscopy while irradiating with Ar-Kα radiation and etching, and using a total detected silicon atom peak area for total peak area of the silicon atom at a binding energy of 102.0 to 104.0 eV,
when X is a proportion (atomic %) in the total detected silicon atom peak area of a peak area at a binding energy of 103.5 to 104.0 eV that corresponds to silicon atoms having a structure given by following (a), and Y is a sum of proportions (atomic %) in the total detected silicon atom peak area of peak areas at a binding energy of 102.0 to 103.4 eV that correspond to silicon atoms having structures given by following formula formulae (b), (c) and (d)
where R1, R2, R3, R4, R5 and R6 independently represent an alkyl group or a phenyl group
(i) Y<X is constantly satisfied in Condition A measurement range described below, and
(ii) a point of transition from Y<X to Y>X is present in Condition B measurement range and Y>X is constantly satisfied after the transition
Condition A:
for a polyethylene terephthalate test specimen, time for which a starting point is time required to erode a depth of 2 nm by irradiation with Ar-Kα radiation and for which an end point is time required to erode a depth of 10 nm, and
Condition B:
for a polyethylene terephthalate test specimen, time for which a starting point is time required to erode a depth of 10 nm by irradiation with Ar-Kα radiation and for which an end point is time required to erode a depth of 20 nm, wherein
0.30≤S4/SA≤0.80
0.00≤S3/SA≤0.50
0.20≤S2/SA≤0.70
when in a chart obtained by 29Si-NMR measurement of the fine particle, SA is a total peak area corresponding to silicon polymer, S4 is a peak area corresponding to formula (a), S3 is a peak area corresponding to formula (b), and S2 is a peak area corresponding to formula (c) where R1, R2 and R3 independently represent an alkyl group having 1 to 6 carbons.

16 more elements

Dependencies are inferred from the claim text.

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Abstract

A fine particle, comprising:

silicon;
the fine particle having a number-average primary particle diameter of 0.05 to 0.30 μm;
the proportion of a silicon atom with reference to a total of elements being at least 20% according to fluorescent x-ray measurement of the fine particle;
and
with respect to the silicon atom proportions measured in analysis by x-ray photoelectron spectroscopy while irradiating with Ar-Kα radiation and etching, and using a total detected silicon atom peak area for total peak area of the silicon atom at a binding energy of 102.0 to 104.0 eV,
when X is a proportion (atomic %) in the total detected silicon atom peak area of a peak area at a binding energy of 103.5 to 104.0 eV that corresponds to silicon atoms having a structure given by following (a), and Y is a sum of proportions (atomic %) in the total detected silicon atom peak area of peak areas at a binding energy of 102.0 to 103.4 eV that correspond to silicon atoms having structures given by following formula formulae (b), (c) and (d)
where R1, R2, R3, R4, R5 and R6 independently represent an alkyl group or a phenyl group
(i) Y<X is constantly satisfied in Condition A measurement range, and
(ii) a point of transition from Y<X to Y>X is present in Condition B measurement range and Y>X is constantly satisfied after the transition
Condition A:
for a polyethylene terephthalate test specimen, time for which a starting point is time required to erode a depth of 2 nm by irradiation with Ar-Kα radiation and for which an end point is time required to erode a depth of 10 nm, and
Condition B:
for a polyethylene terephthalate test specimen, time for which a starting point is time required to erode a depth of 10 nm by irradiation with Ar-Kα radiation and for which an end point is time required to erode a depth of 20 nm, wherein
0.30≤S4/SA≤0.80
0.00≤S3/SA≤0.50
0.20≤S2/SA≤0.70
when in a chart obtained by 29Si-NMR measurement of the fine particle, SA is a total peak area corresponding to silicon polymer, S4 is a peak area corresponding to formula (a), S3 is a peak area corresponding to formula (b), and S2 is a peak area corresponding to formula (c) where R1, R2 and R3 independently represent an alkyl group having 1 to 6 carbons.

14 more elements