Classifications

• • G—PHYSICS
  • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
  • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
  • G03G9/00—Developers
  • G03G9/08—Developers with toner particles
  • G03G9/097—Plasticisers; Charge controlling agents
  • G03G9/09708—Inorganic compounds
• • G—PHYSICS
  • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
  • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
  • G03G9/00—Developers
  • G03G9/08—Developers with toner particles
  • G03G9/087—Binders for toner particles
  • G03G9/08742—Binders for toner particles comprising macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • G03G9/08755—Polyesters
• • G—PHYSICS
  • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
  • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
  • G03G9/00—Developers
  • G03G9/08—Developers with toner particles
  • G03G9/087—Binders for toner particles
  • G03G9/08784—Macromolecular material not specially provided for in a single one of groups G03G9/08702 - G03G9/08775
  • G03G9/08797—Macromolecular material not specially provided for in a single one of groups G03G9/08702 - G03G9/08775 characterised by their physical properties, e.g. viscosity, solubility, melting temperature, softening temperature, glass transition temperature
• • G—PHYSICS
  • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
  • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
  • G03G9/00—Developers
  • G03G9/08—Developers with toner particles
  • G03G9/097—Plasticisers; Charge controlling agents
  • G03G9/09708—Inorganic compounds
  • G03G9/09716—Inorganic compounds treated with organic compounds
• • G—PHYSICS
  • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
  • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
  • G03G9/00—Developers
  • G03G9/08—Developers with toner particles
  • G03G9/097—Plasticisers; Charge controlling agents
  • G03G9/09708—Inorganic compounds
  • G03G9/09725—Silicon-oxides; Silicates

Definitions

• a toner particle according to an example includes a core particle, first inorganic particles externally added to the core particle, and second inorganic particles externally added to the core particle.
• the core particle includes, for example, a binder resin.
• the binder resin includes, for example, one or more amorphous polyester resins and one or more crystalline polyester resins.
• the amorphous polyester resin may be a polyester resin exhibiting no distinct endothermic peak in a differential scanning calorimetry (DSC) curve.
• the amorphous polyester resin may be defined as, for example, a polyester resin exhibiting a stepwise endothermic change when measured at a temperature increase rate of 10 °C/min by differential scanning calorimetry, or a polyester resin exhibiting an endothermic peak with a half width of more than 15°C.
• An amorphous polyester resin is, for example, a reaction product of a polyhydric alcohol and a polycarboxylic acid.
• the amorphous polyester resin includes, as monomer units, a polyhydric alcohol and a polycarboxylic acid.
• the polyhydric alcohol may be, for example, a diol.
• the diol include aliphatic diols such as ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, butanediol, hexanediol, neopentyl glycol, and glycerin; alicyclic diols such as cyclohexanediol, cyclohexanedimethanol, and hydrogenated bisphenol A; and aromatic diols such as an ethylene oxide adduct of bisphenol A and a propylene oxide adduct of bisphenol A.
• These polyhydric alcohols may be used singly or in combination of two or more kinds thereof.
• the diol may be an aromatic diol in some examples, or an alicyclic diol in other examples.
• the polyhydric alcohol may further include, in addition to a diol, a polyhydric alcohol having a valency of 3 or more (for example, glycerin, trimethylolpropane, or pentaerythritol).
• the content of the polyhydric alcohol may be 50% by mole or more, 55% by mole or more, or 60% by mole or more, and may be 80% by mole or less, 75% by mole or less, or 70% by mole or less, based on the total amount of the monomer units in the amorphous polyester resin.
• the polycarboxylic acid may include, for example, an aromatic polycarboxylic acid having an aromatic ring, and may include an anhydride of the aromatic polycarboxylic acid.
• the polycarboxylic acid may include, for example, an aromatic dicarboxylic acid, and may include an anhydride of an aromatic dicarboxylic acid.
• polycarboxylic acid examples include phthalic acid, isophthalic acid, terephthalic acid, tetrachlorophthalic acid, chlorophthalic acid, nitrophthalic acid, p-carboxyphenylacetic acid, p- phenylene-2-acetic acid, m-phenylene diglycolic acid, p-phenylene diglycolic acid, o-phenylene diglycolic acid, diphenylacetic acid, diphenyl-p,p' ⁇ dicarboxylic acid, naphthalene-1 ,4-dicarboxylic acid, naphthalene-1 ,5- dicarboxylic acid, naphthalene-2,6-dicarboxylic acid, anthracene dicarboxylic acid, and anhydrides of these. These polycarboxylic acids may be used singly or in combination of two or more kinds thereof.
• the polycarboxylic acid may further include, for example, an aromatic polycarboxylic acid having 3 or more valences, and may further include an anhydride of an aromatic polycarboxylic acid having 3 or more valences.
• examples of the polycarboxylic acid include trimellitic acid, pyromellitic acid, naphthalenetricarboxylic acid, naphthalenetetracarboxylic acid, pyrenetricarboxylic acid, pyrenetetracarboxylic acid, and acid anhydrides of these carboxylic acids.
• the content of the polycarboxylic acid may be 20% by mass or more, 25% by mass or more, or 30% by mass or more, and may be 50% by mass or less, 45% by mass or less, or 40% by mass or less, based on the total mass of the monomer units in the amorphous polyester resin.
• the weight average molecular weight of the amorphous polyester resin may be 5,000 or more, 10,000 or more, or 12,000 or more, and may be 50,000 or less, 45,000 or less, or 40,000 or less, depending on examples.
• the weight average molecular weight of the amorphous polyester resin according to the present disclosure is measured according to gel permeation chromatography (GPC) of a tetrahydrofuran (THF)-soluble fraction.
• GPC gel permeation chromatography
• the weight average molecular weight may be determined by the following method. Waters e2695 (manufactured by Nihon Waters K.K.) is used as a measuring apparatus, and two sets of Snertsil CN-3 25 cm (manufactured by GL Sciences, Inc.) are used as columns.
• THF tetrahydrofuran
• the sample solution is injected into the measuring apparatus in an amount of 20 uL, and measurement is made under the conditions of 40°C and a flow rate of 1.0 mL/min.
• the glass transition temperature (Tg) of the amorphous polyester resin may be 50°C or more, and may be 80°C or less or 70°C or less, depending on examples.
• the content of the first amorphous polyester resin may be 60% by mass or more, 70% by mass or more, or 80% by mass or more, and may be 95% by mass or less, 92% by mass or less, or 90% by mass or less, based on the total mass of the binder resin.
• the content of the amorphous polyester resin may be 50% by mass or more, 55% by mass or more, or 60% by mass or more, and may be 90% by mass or less, 85% by mass or less, or 80% by mass or less, based on the total mass of the toner particle.
• the crystalline polyester resin may be a polyester resin exhibiting a clear endothermic peak in a modified differential scanning calorimetry (MDSC) curve.
• MDSC modified differential scanning calorimetry
• a crystalline polyester resin is, for example, a reaction product between a polyhydric alcohol and a polycarboxylic acid.
• a crystalline polyester resin includes a polyhydric alcohol and a polycarboxylic acid as monomer units.
• the polyhydric alcohol may be, for example, a diol or an aliphatic diol.
• the number of carbon atoms of the polyhydric alcohol may be 8 or more or 9 or more, and may be 12 or less or 10 or less, depending on examples. Accordingly, the number of carbon atoms of the polyhydric alcohol may be 9 in some example, or 10 in other examples.
• Examples of the polyhydric alcohol include 1 ,9-nonanediol.
• the content of the polyhydric alcohol may be 30% by mass or more, 35% by mass or more, or 40% by mass or more, and may be 60% by mass or less, 55% by mass or less, or 50% by mass or less, based on the total mass of monomer units in the crystalline polyester resin.
• the polycarboxylic acid may be, for example, an aliphatic polycarboxylic acid.
• the aliphatic polycarboxylic acid may be an aliphatic dicarboxylic acid in order to increase linearity of the structure of the crystalline polyester resin increases, so as to increase the affinity with the amorphous polyester resin.
• the number of carbon atoms of the polycarboxylic acid may be 8 or more or 9 or more, and may be 12 or less or 10 or less, depending on examples.
• the number of carbon atoms may be 9 in some examples, or 10 in other examples.
• the polycarboxylic acid include 1 ,10-decane dicarboxylic acid and 1 ,12-dodecane dicarboxylic acid.
• the content of the polycarboxylic acid may be 40% by mass or more, 45% by mass or more, or 50% by mass or more, and may be 70% by mass or less, 65% by mass or less, or 60% by mass or less, based on the total mass of monomer units in the crystalline polyester resin.
• the weight average molecular weight of the crystalline polyester resin may be 5,000 or more, 5,500 or more, or 6,000 or more, and may be 15,000 or less, 10,000 or less, or 8,000 or less, depending on examples.
• the weight average molecular weight of the crystalline polyester resin is measured by the same method as that for the weight average molecular weight of the amorphous polyester resin.
• the melting temperature (Tm) of the crystalline polyester resin may be 60°C or more and may be 100°C or less or 75 c C or less, depending on examples.
• the content of the crystalline polyester resin may be 5% by mass or more, 8% by mass or more, or 10% by mass or more, and may be 40% by mass or less, 30% by mass or less, or 20% by mass or less, based on the total mass of the binder resin.
• the content of the crystalline polyester resin may be 3% by mass or more, 5% by mass or more, or 8% by mass or more, and may be 30% by mass or less, 20% by mass or less, or 15% by mass or less, based on the total mass of the toner particle.
• the binder resin may further include other resins in addition to the amorphous polyester resin and crystalline polyester resin.
• the other resins include a styrene-(meth)acrylic copolymer, an epoxy resin, and a styrene-butadiene copolymer.
• the styrene-(meth)acrylic copolymer may be a copolymer of a styrene-based monomer and a (meth)acrylic acid ester- based monomer.
• Examples of the styrene-based monomer include styrene, o- (m-, p-) methylstyrene and m- (p ⁇ ) ethylstyrene.
• Examples of the (meth)acrylic acid ester-based monomer include methyl (meth)acrylate, ethyl (meth)acrylate, propyl (meth)acrylate, butyl (meth)acrylate, octyl (meth)acrylate, dodecyl (meth)acrylate, stearyl (meth)acrylate, behenyl (meth)acrylate, 2-ethylhexyl (meth)acrylate, dimethylaminoethyl (meth)acrylate, and diethylaminoethyl (meth)acrylate.
• the total content of the amorphous polyester resin and crystalline polyester resin in the binder resin may be 80% by mass or more, 85% by mass or more, or 90% by mass or more, and may be 98% by mass or less or 95% by mass or less, based on the total mass of the binder resin.
• the content of the binder resin in the toner particle may be 40% by mass or more, 45% by mass or more, or 50% by mass or more, and may be 90% by mass or less, 85% by mass or less, or 75% by mass or less, based on the total mass of the toner particle.
• the core particle may further include a colorant.
• the colorant can include at least one colorant selected from, for example, a black colorant, a cyan colorant, a magenta colorant, and a yellow colorant.
• a black colorant e.g., a black colorant, a cyan colorant, a magenta colorant, and a yellow colorant.
• the colorant one kind may be used alone, or two or more kinds thereof may be used as a mixture, in consideration of hue, chroma, brightness, weatherresistance, dispersibility in toner, and the like.
• the black colorant may be carbon black or aniline black.
• the yellow colorant may be a condensed nitrogen compound, an isoindolinone compound, an anthraquine compound, an azo metal complex, or an allylimide compound.
• Some examples of the yellow colorant include C.l. Pigment Yellow 12, 13, 14, 17, 62, 74, 83, 93, 94, 95, 109, 110, 111 , 128, 129, 147,
• the magenta colorant may be a condensed nitrogen compound, anthraquine, a quinacridone compound, a basic dye lake compound, a naphthol compound, a benzimidazole compound, a thioindigo compound, or a perylene compound.
• Some examples of the magenta colorant include C.l. Pigment Red 2, 3, 5, 6, 7, 23, 48:2, 48:3, 48:4, 57:1 , 81 :1 , 122, 144, 146, 166,
• the cyan colorant may be a copper phthalocyanine compound or a derivative thereof, an anthraquine compound, or the like.
• Some examples of the cyan colorant include C.l. Pigment Blue 1 , 7, 15, 15:1 , 15:2, 15:3, 15:4, 60, 62, and 66.
• the content of the colorant may be 0.5% by mass or more, 1 % by mass or more, or 2% by mass or more, based on the total mass of the toner particle, in order to achieve a sufficient coloration effect, and the content of the colorant may be 15% by mass or less, 12% by mass or less, or 10% by mass or less, based on the total mass of the toner particle, in order to achieve a sufficient amount of frictional electrification without having significant influence on the increase in the production cost of the toner particle.
• the core particle may further include a release agent. Since the release agent promotes low-temperature fixability, final image durability, and abrasion resistance of the toner particles, the type and content of the release agent may be determined in consideration of the properties of the toner.
• the release agent may include, for example, a wax.
• the wax may be a natural wax or a synthetic wax.
• the wax can be selected, for example, from the group consisting of polyethylene wax, polypropylene wax, silicon wax, paraffin wax, ester wax, carnauba wax, beeswax, and metallocene wax.
• the content of the release agent may be 1 % by mass or more, 2% by mass or more, or 3% by mass or more, , based on the total mass of the toner particle, in order to achieve a suitable low- temperature fixability and a sufficient fixing temperature range, and may be 20% by mass or less, 15% by mass or less, or 10% by mass or less, based on the total mass of the toner particle, in order to achieve suitable storage stability and economic efficiency.
• the content of the core particles may be 80% by mass or more, 85% by mass or more, or 90% by mass or more, and may be 99% by mass or less, 98% by mass or less, or 97% by mass or less, based on the total mass of the toner particles.
• the average particle diameter of the core particle may be 3 pm or more, 4 pm or more, or 5 pm or more, and may be 12 pm or less, 11 pm or less, 10 pm or less, or 9 pm or less, depending on examples.
• the average particle diameter of the core particle is measured by the method described further below with reference to Test Examples.
• the core particle may include a central portion including an amorphous polyester resin and a crystalline polyester resin as the binder resin, and a coating portion coating the central portion and including an amorphous polyester resin as the binder resin.
• the average diameter of the central portion may be 2.8 pm or more, 3.5 pm or more, or 4 pm or more, and may be 11 pm or less, 10 pm or less, or 9 pm or less, depending on examples.
• the average diameter of the central portion is measured by the method described further below with reference to the Test Examples.
• the thickness of the coating portion may be 0.2 pm or more, 0.4 pm or more, or 0.5 pm or more, and may be 2.0 pm or less, 1 .4 pm or less, or 0.8 pm or less, depending on examples.
• the first and second inorganic particles externally added to the core particle are attached to the surface of the core particle.
• the first inorganic particles and the second inorganic particles are different inorganic particles from each other.
• the first inorganic particles have a true density of 3.0 g/cm 3 or less.
• the true density of the first inorganic particles may be 2.8 g/cm 3 or less, 2.5 g/cm 3 or less, 2.3 g/cm 3 or less, or 2.1 g/cm 3 or less, or may be 1.7 g/cm 3 or more.
• the true density of the first inorganic particles is measured by the method described in Examples.
• the first inorganic particles have an average particle diameter of 30 nm or less.
• the average particle diameter of the first inorganic particles may be 25 nm or less, 20 nm or less, or 15 nm or less, or may be 7 nm or more, depending on examples.
• the average particle diameter of the first inorganic particles is measured by the method described further below with reference to the Test Examples.
• the second inorganic particles have a dielectric constant of 1 .0 * 10 2 or less.
• the dielectric constant of the second inorganic particles may be 8.0 x 10 1 or less, 7.0 x 10 ' or less, 6.0 x 10 1 or less, or 5.0 x 10 1 or less, or may be 1 .0 * 10 1 or more, depending on examples.
• the dielectric constant of the second inorganic particles is measured by the method described further below with reference to the Test Examples.
• the ratio of the true density of the second inorganic particles to the true density of the first inorganic particles is greater than 1 and no greater than 1.5.
• the true density ratio may be 1.05 or more, 1.1 or more, 1 .2 or more, or 1 .3 or more, depending on examples.
• the true density ratio may be 1.8 cr less, 1.7 or less, 1.6 or less, cr 1.5 or less, depending on examples.
• the true density of the second inorganic particles is measured by the method described further below with reference to the Test Examples.
• the ratio of the dielectric tangent of the second inorganic particles to the dielectric tangent of the first inorganic particles is 3 or more.
• the ratio of the dielectric tangent may be 5 or more, 10 or more, 20 or more, 30 or more, 40 or more, 50 or more, or 60 or more, and may be 80 or less, 70 or less, 65 or less, or 50 or less, depending on examples.
• the dielectric tangent of the first and second inorganic particles is measured by the methods described further below with reference to the Test Examples.
• first and second inorganic particles is appropriately selected from inorganic particles satisfying the above-described characteristics.
• the dielectric constant of the first inorganic particles may be, for example, 3.0 x 10 1 or more, 4.0 x 10 1 or more, or 4.5 x 10 1 or more, and may be 7.0 x 1 o 1 or less, 6.0 x io 1 or less, or 5.5 x 10 1 or less, depending on examples.
• the dielectric constant of the first inorganic particles is measured by the method described further below with reference to the Test Examples.
• the dielectric tangent of the first inorganic particles may be a value that satisfies the above dielectric tangent ratio, and may be, for example, 1.0 x 10 -3 or more, 1 .2 x 1O ⁇ 3 or more, or 1 .5 x 1O ⁇ 3 or more, and may be 5.0 x w 3 or less, 3.0 x w 3 or less, or 2.0 x 1O‘ 3 or less, depending on examples.
• the average particle diameter of the second inorganic particles may be 50 nm or less, 40 nm or less, or 30 nm or less, and may be 5 nm or more, 10 nm or more, or 15 nm or more, depending on examples.
• the average particle diameter of the second inorganic particles is measured by the method described further below with reference to the Test Examples.
• the true density of the second inorganic particles may be a value that satisfies the above true density ratio, and may be, for example, 2.0 g/cm 3 or more, 2.1 g/cm 3 or more, 2.2 g/cm 3 or more, or 2.3 g/cm 3 or more, and may be 3.5 g/cm 3 or less, depending on examples.
• the dielectric tangent of the second inorganic particles may be a value that satisfies the above dielectric tangent ratio, and may be, for example, 5.0 x w 3 or more, 3.0 x w 2 or more, or 5.0 x w 2 or more, and may be 2.0 x 10' 1 or less, 1.5 x w 2 or less, or 1.0 x 10' 2 or less, depending on examples.
• the dielectric constant of the second inorganic particles is measured by the method described further below with reference to the Text Examples.
• the first inorganic particles may be, for example, SiOa particles containing SiO2.
• the S1O2 particles satisfying the characteristics of the first inorganic particles described above can be obtained, for example, by purchasing a commercially available product.
• the first inorganic particles may further contain a metal oxide in addition to SiO2.
• the metal oxide may be AI2O3.
• the first inorganic particles may be S1O2/AI2O3 composite particles containing S1O2 and AI2O3.
• the second inorganic particles may be, for example, composite particles containing SiOa and a metal oxide.
• the metal oxide may be AI2O3.
• the second inorganic particles may be SiO 2 /AI 2 O 3 composite particles containing S1O2 and AI2O3.
• the metal oxide may be ZrCh.
• the second inorganic particles may be SifMZrCh composite particles containing SiO2 and ZrCh.
• the metal oxide may be T1O2.
• the second inorganic particles may be SiCh/TiCh composite particles containing SiOz and TiCh.
• the composite particles satisfying the characteristics of the second inorganic particles described above can be obtained by a synthesizing method for example, as described further below with reference to the Test Examples.
• the content (addition amount) of the first inorganic particles may be 0.05 parts by mass or more, 0.1 parts by mass or more, or 0.2 parts by mass or more, and may be 3 parts by mass or less, 2 parts by mass or less, or 1 part by mass or less, based on 100 parts by mass of the core particle.
• the content (addition amount) of the second inorganic particles may be 0.1 parts by mass or more, 0.4 parts by mass or more, or 0.7 parts by mass or more, and may be 3 parts by mass or less, 2 parts by mass or less, or 1.5 parts by mass or less, based on 100 parts by mass of the core particle.
• the toner particle may further include other inorganic particles not corresponding to the first inorganic particles and the second inorganic particles.
• Other inorganic particles may be externally added to the core particle.
• the other inorganic particles may be, for example, S1O2 particles having an average particle diameter of more than 30 nm.
• the average particle diameter of the SiO2 particles may be 35 nm or more, or 40 nm or more.
• the content (addition amount) of the other inorganic particles may be 0.5 parts by mass or more, 0.8 parts by mass or more, or 1 part by mass or more, and may be 3 parts by mass or less, 2 parts by mass or less, or 1 .5 parts by mass or less, based on 100 parts by mass of the core particle.
• the toner particle may further contain a charge control agent, in some examples.
• the charge control agent may be internally added so as to be contained in the core particle, or may be externally added so as to attach to the surface of the core particle.
• the charge control agent may be a negative charge control agent or a positive charge control agent.
• Examples of the negative charge control agent include a salicylic acid metal compound, a naphthoic acid metal compound, a dicarboxylic acid metal compound, a polymer type compound having sulfonic acid or carboxylic acid in a side chain, a polymer type compound having a sulfonic acid salt or a sulfonic acid esterification product in a side chain, a polymer type compound having a carboxylic acid salt or a carboxylic acid esterification product in a side chain, a boron compound, a urea compound, a silicon compound, and a calixarene.
• Examples of the positive charge control agent include a quaternary amount salt, a polymer type compound having a quaternary ammonium salt in a side chain, a guanidine compound, and an imidazole compound.
• the average particle diameter of the toner particles may be, for example, 3 pm or more, 4 pm or more, or 5 pm or more, and may be 12 pm or less, 11 pm or less, 10 pm or less, or 9 pm or less.
• the average particle diameter of the toner particles is measured by the method described further below with reference to the Test Examples.
• the toner particle described above are obtained by a producing method according to examples of the present disclosure, including a step of externally adding the first inorganic particles and the second inorganic particles to the core particle.
• the first inorganic particles and the second inorganic particles may be externally added to the core particles by mixing the core particle, the first inorganic particles and the second inorganic particles with a powder mixer.
• the toner particle can be used as a one-component system developer.
• the toner particle can be mixed with a magnetic carrier and used as a two-component system developer.
• Examples of the magnetic carrier include: iron oxide; metal particle such as iron, lithium, calcium, magnesium, nickel, copper, zinc, cobalt, manganese, chrome, and rare earth elements; particle of alloys thereof, particle of oxides thereof; magnetic bodies such as ferrites; and a magnetic body-dispersed resin carrier (that may be referred to as a resin carrier) containing a magnetic body and a binder resin that maintains the magnetic body in a dispersed state.
• a resin carrier that may be referred to as a resin carrier
• the content of the toner particle may be 2% by mass or more or 4% by mass or more, and may be 15% by mass or less or 13% by mass or less, based on the total mass of the two-component system developer.
• the toner particle may be accommodated in, for example, a toner cartridge.
• the toner particle may be accommodated within a container in a toner cartridge.
• a toner cartridge including a container that accommodates the example toner particle described above.
• toner particle will be described by way of Test Examples, although the toner particle is not limited to the Test Examples described.
• terephthalic acid 30.4 parts by mass of terephthalic acid, 1.1 parts by mass of trimellitic anhydride, 67.3 parts by mass of BP-2P (trade name, bisphenol A propylene oxide 2 mol adduct, manufactured by Sanyo Chemical Industries, Ltd.), 1.2 parts by mass of ethylene glycol, and 1.0 parts by mass of dibutyltin oxide (catalyst) were introduced in a 500 ml four-necked flask equipped with a nitrogen inlet tube, a dehydration tube, a stirrer, and a thermocouple.
• BP-2P trade name, bisphenol A propylene oxide 2 mol adduct, manufactured by Sanyo Chemical Industries, Ltd.
• the mixture was heated to 230 °C under a nitrogen atmosphere, and reacted until the reaction rate reached 90%, and then reacted at 8.3 kPa until the targeted weight average molecular weight was reached, thereby obtaining amorphous polyester resin 1 .
• the weight average molecular weight Mw and the glass transition temperature Tg of the amorphous polyester resin 1 were measured by the methods described further below.
• the amorphous polyester resin 1 had Mw of 11 ,400 and Tg of 59 °C.
• amorphous polyester resin 2 30.5 parts by mass of terephthalic acid, 1.0 parts by mass of trimellitic anhydride, 68.1 parts by mass of BP-2P, 0.4 parts by mass of ethylene glycol, and 1.0 parts by mass of dibutyltin oxide (catalyst) were introduced in a 500 ml four-necked flask equipped with a nitrogen inlet tube, a dehydration tube, a stirrer, and a thermocouple. The mixture was heated to 230 °C under a nitrogen atmosphere, and reacted until the reaction rate reached 90%, and then reacted at 8.3 kPa until the targeted weight average molecular weight was reached, thereby obtaining amorphous polyester resin 2.
• the weight average molecular weight Mw and the glass transition temperature Tg of the amorphous polyester resin 2 were measured by the methods described further below.
• the amorphous polyester resin 2 had Mw of 40,300 and Tg of 58 °C.
• the weight average molecular weight Mw was determined by gel permeation chromatography (GPC) measurement. Namely Waters e2695 (manufactured by Nihon Waters K. K.) was used as a measuring apparatus, and Inertsil CN-3 25 cm two series (manufactured by GL Sciences Inc.) were used as a column. In addition, 30 mg of the polyester resin was added to 20 mL of tetrahydrofuran (THF) (containing a stabilizer, manufactured by Wako Pure Chemical Industries, Ltd.), stirred for 1 hour, and then filtered with a 0.2 pm filter to obtain a filtrate, which was used as a sample solution. The tetrahydrofuran (THF) sample solution (20 pL) was injected into the measurement apparatus, and measurement was performed under the conditions of 40°C and a flow rate of 1 .0 mL/min.
• GPC gel permeation chromatography
• the glass transition temperature Tg was determined from a differential scanning calorimetry curve obtained by differential scanning calorimetry measurement specified in ASTM D3418-08. Namely, using a DSC Q2000 (manufactured by TA Instruments), the temperature was raised from room temperature to 150°C at a rate of 10°C per minute as a first temperature raising step, and after holding at 150°C for 5 minutes, the temperature was lowered to 0°C at a rate of 10°C per minute by liquefied nitrogen. Then, after holding at 0°C for 5 minutes, the temperature was raised again from 0°C to 150°C at a rate of 10°C per minute as a second temperature raising step, and the glass transition temperature was determined from the obtained DSC curve.
• the melting point Tm was determined from a differential scanning calorimetry curve obtained by differential scanning calorimetry (DSC) as defined in ASTM D341-08. Namely, using a DSC Q2000 (manufactured by TA Instruments), the temperature was raised from room temperature to 150°C at a rate of 10°C per minute as a first temperature raising step, and after holding at 150°C for 5 minutes, the temperature was lowered to 0°C at a rate of 10°C per minute by liquefied nitrogen.
• DSC differential scanning calorimetry
• the temperature was raised again from 0°C to 150°C at a rate of 10°C per minute as a second temperature raising step, and the heat absorption peak temperature at the time of melting of the crystalline polyester resin was taken as Tm from the obtained DSC curve.
• amorphous polyester resin 1 400g of the amorphous polyester resin 1 , 600g of methylethylketone, and 100g of isopropyl alcohol were introduced into a double jacket reaction vessel, and 30g of 5% aqueous ammonia solution was gradually added to the mixture while the mixture was stirred with a semi-moon type impeller at about 30 °C. Then, while stirring was continued, 1500g of water was added at a rate of 20 g/min to prepare an emulsion. The solvent was removed from the prepared emulsion by vacuum distillation to obtain amorphous polyester resin latex 1 having a solid content of 20%.
• amorphous polyester resin 2 400g of the amorphous polyester resin 2, 500g of methylethylketone, and 200g of isopropyl alcohol were introduced into a double jacket reaction vessel, and 30g of 5% aqueous ammonia solution was gradually added to the mixture while the mixture was stirred with a semi-moon type impeller at about 30 °C. Then, while stirring was continued, 1500g of water was added at a rate of 20 g/min to prepare an emulsion. The solvent was removed from the prepared emulsion by vacuum distillation to obtain amorphous polyester resin latex 2 having a solid content of 20%.
• the temperature of the aggregation reaction liquid was increased at a rate of 0.03 °C/min to continue the aggregation reaction, thereby obtaining primary aggregated particles (central portions) having a volume average particle diameter of 4 to 5 pm.
• 300g of a mixture obtained by mixing the amorphous polyester resin latex 1 and the amorphous polyester resin latex 2 at a mass ratio of 1 :1 was further added to the reaction vessel, followed by coagulation for 0.5 hours.
• a 1 N NaOH aqueous solution was added to adjust the pH to 7.5 or more and 9 or less.
• the temperature was increased to a temperature of 80 °C to 90 °C, and fusion was performed for 3 to 5 hours to obtain secondary aggregated particles (core particles) having a volume average particle diameter of 5 to 7 pm.
• the aggregation reaction solution was cooled to 28 °C or less, and then filtered to separate and dry the particles, thereby obtaining core particles having a central portion and a coating portion on the outer surface thereof.
• the volume average particle diameter of the obtained core particles was 6 pm.
• the volume average particle diameter of each of the primary aggregated particles and the secondary aggregated particles was measured by the following method by taking out a part of the mixed solution from the reaction vessel and collecting the primary or secondary aggregated particles contained in the solution.
• a Coulter counter manufactured by Beckman Coulter, Inc.
• ISOTON II manufactured by Beckman Coulter, Inc.
• measurement was performed under the condition of a measured particle number of 30,000 using an aperture tube having an aperture diameter of 100 pm.
• the volumes occupied by the particles included in the divided particle size ranges are accumulated from the small diameter side, and the size at which the accumulation is 50% is defined as a volume average particle diameter Dv50.
• 300g of tetramethoxysilane, 700g of methanol, 35g of a 20% aqueous ammonia solution, and 105g of water were introduced into a 3L double-jacket reaction vessel. Under an environment of about 30 °C, the content in the reaction vessel was stirred with a semi-moon type impeller to obtain SiCh slurry. At about 70 °C, 5N NaOH aqueous solution was gradually added to the SiO 2 slurry to adjust the pH of the mixture to about 9.0. Subsequently, 30g of sodium aluminate was added, and then a 5N NaOH aqueous solution was gradually added to adjust the pH to about 6.0.
• the content in the reaction vessel was stirred with a semi-moon type impeller in an environment of about 80 °C to obtain SiOa/AhOs slurry.
• the obtained SiOs/AhOa slurry was dried, and then the solid was disintegrated to obtain precursor of SiCh/AhCh composite particles.
• 100g of the obtained precursor was introduced in a reaction vessel, 10g of isobutylmethoxysilane and 60 ml of n-hexane were added thereto, and the mixture was stirred at room temperature for 30 minutes. Subsequently, the mixture was heated to about 200 °C, stirred for 60 minutes, and then cooled to room temperature to obtain SiOz/AhOs composite particles 1 .
• SiOs/AbOs composite particles 2 were obtained in a similar manner as the SiOs/AbCh composite particles 1 with the difference that the addition amount of sodium aluminate was changed to 55g. [0079] Synthesis of S1O2/AI2O3 composite particles 3
• SiCh/AhCh composite particles 3 were obtained in a similar manner as the S1O2/AI2O3 composite particles 1 with the difference that the addition amount of sodium aluminate was changed to 78g.
• SiCh/AhCh composite particles 4 were obtained in a similar manner as the S1O2/AI2O3 composite particles 1 with the difference that the addition amount of sodium aluminate as changed to 6g.
• SiOs/AhOs composite particles 5 were obtained in a similar manner as the SiOs/AbCh composite particles 1 with the difference that the addition amount of sodium aluminate was changed to 1 ,5g.
• SiO2/ZrO2 composite particles 1 were obtained in a similar manner as the SiO2/Al2Os composite particles 1 with the difference that the sodium aluminate was changed to zirconium sulfate and the addition amount was changed to 120g.
• SiOa/ZrCh composite particles 2 were obtained in a similar manner as the SiO2/'ZrO2 composite particles 1 with the difference that the addition amount of zirconium sulfate was changed to 240g.
• SiO2 particles As SiO2 particles, AI2O3 particles, and HO2 particles, the following were used.
• S1O2 particles 1 R8200, manufactured by Aerosil
• SiOs particles 2 X24-9404E, manufactured by Shin-Etsu Chemical
• SiOa particles 3 H2000, manufactured by Clariant S1O 2 particles 4: NY 50, manufactured by Aerosil
• AI 2 O 3 partides NA - 100B, manufactured by Titan Kogyo
• TiO 3 particles STT-2S, manufactured by Titan Kogyo
• the volume-based median diameter (Dv50) of each of the inorganic particles was measured as average particle diameter. The results are shown in Tables 2 and 3.
• each of the inorganic particles was measured by a gas displacement method using a dry automatic densimeter (Accupyc 1330, manufactured by Shimadzu Corporation). Namely, each of the inorganic particles was filled in a sample cell of 10cm 3 ( ⁇ p18.5 * 39.5 mm), purged 10 times with helium gas, and then measured 10 times continuously at room temperature (23 ⁇ 3 °C). The results are shown in Tables 2 and 3.
• each of the inorganic particle was filled in a measurement cell, and a load of about 6 kN was applied by a sample hydraulic press to prepare the measurement sample having a thickness of 1 .0 ⁇ 0.5 mm.
• the measurement apparatus includes:
• Electrode cell for powder manufactured by SUS
• the measured values were regarded as measured values of a composite of the inorganic particles (powder) and air, and £ r and tan 6 of the inorganic particles (powder) themselves were calculated using a relationship based on the logarithmic mixing rule according to the following formula: wherein £ c is the complex dielectric constant of the composite, is the complex dielectric constant of the inorganic particles (powder), £b is the complex dielectric constant of air, and $ is the volume fraction of the inorganic particles (powder) in the sample cell (bulk density of the composite / true density of the inorganic particles (powder)).
• Each of the obtained toner particles was evaluated for chargeability by the foilowing method.
• the toner particle and a ferrite carrier (average particle diameter: 40 pm, manufactured by Kanto Denka Kogyo Co., Ltd.) were introduced into a 50 ml polymer container in a total amount of 20g (the proportion of the toner particles was 7% by mass) to obtain a mixture of the toner particle and the ferrite carrier.
• the mixture was left to stand in a low-temperature and low- humidity environment (10°C/10%RH) for 24 hours, and then a sample was taken every 10 seconds while stirring with a Turbula mixier T2F type (manufactured by Willy A. Bachofen AG), and the toner average charge amount: Q/M (pC/g) was measured by a suction-type Faraday cage method. Namely, the sample was directly suctioned by a suction pump and collected by the Faraday cage containing a filter paper. The charge amount of the sample collected on the filter paper was measured by a q/m Meter Model 210- HS manufactured by Treck Corporation connected to the Faraday cage.
• the toner average charge amount Q/M (pC/g) was calculated from the mass M of the collected toner particles and the charge amount Q thereof. The measurement of Q/M was carried out for 1 hour, and the highest Q/M value (peak value) in the period and the Q/M value after 20 seconds from the start of stirring were calculated. The ratio (%) of the value of Q/M after 20 seconds from the start of stirring to the peak value of Q/M is shown in Tables 2 and 3 as an index of the charge rising property. The greater the ratio, the better the charge rising property. In some examples, the ratio may be 25% or more. [0093] Charge retention property
• the Q/M after 1 hour from the start of stirring was measured in a similar manner as in the charge rising property with the difference that the Sowtemperature and Sow-humidity environment (10°C/10%RH) was changed to a high-temperature and high-humidity environment (30°C/80%RH). Subsequently, the stirring was stopped and the mixture was left to stand for 20 hours, after which the Q/M was measured.
• Q/M after standing for 20 hours to the peak value of Q/M after 1 hour from the start of stirring is shown in Tables 2 and 3 as an index of charge retention property.
• example toner particles can achieve both suitable charge rising property and charge retention property by using a combination of the example first and second inorganic particles.

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