CN100522824C - Method for preparing Nano particles of monodisperse, ultra paramagnetic ferroferric oxide - Google Patents

Method for preparing Nano particles of monodisperse, ultra paramagnetic ferroferric oxide Download PDF

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CN100522824C
CN100522824C CNB2007100482663A CN200710048266A CN100522824C CN 100522824 C CN100522824 C CN 100522824C CN B2007100482663 A CNB2007100482663 A CN B2007100482663A CN 200710048266 A CN200710048266 A CN 200710048266A CN 100522824 C CN100522824 C CN 100522824C
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water
monodisperse
nano particles
ferroferric oxide
preparation
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CN101003389A (en
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温贤涛
顾忠伟
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Sichuan University
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Sichuan University
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Abstract

This invention discloses a method for preparing monodisperse superparamagnetic Fe3O4 nanoparticles. The method comprises: (1) mixing soluble Fe3+ salt, soluble Fe2+ salt, anionic surfactant, and mixed solvents of water and organic solvent; (2) adding into a reactor under nitrogen protection, stirring until the solids are completely dissolved and water-insoluble organic phase turns into brown, heating to refluxing temperature, and refluxing for 10 min-4 h; (3) cooling to room temperature after refluxing, adding separating agent to precipitate Fe3O4 particles, separating Fe3O4 particles from the solvent, washing, and drying in a vacuum oven to obtain monodisperse monodisperse superparamagnetic Fe3O4 nanoparticles.

Description

The preparation method of Nano particles of monodisperse, ultra paramagnetic ferroferric oxide
Technical field
The invention belongs to Z 250 (Fe 3O 4) nanometer particle process method, particularly a kind of monodisperse, ultra paramagnetic ferroferric oxide (Fe that dissolves in non-polar solvent 3O 4) nanometer particle process method.
Background technology
Super paramagnetic effect is a kind of special magnetic property, and the material with superparamagnetism is magnetized when being in the externally-applied magnetic field, but after externally-applied magnetic field was decorporated, the super paramagnetic material specific magnetising moment was almost nil, and coercive force is very little.Because this character, super paramagnetic material is applied to many fields.Therefore, super paramagnetic material, the preparation of particularly monodispersed super paramagnetic nano particle receives publicity always.
The method for preparing Z 250 has following several: chemical coprecipitation, and with Fe 3+And Fe 2+Soluble salt soluble in water in the 2:1 ratio, under nitrogen protection, drip alkaline solution such as NaOH or NH then 3H 2O makes Fe 3+And Fe 2+Be precipitated out and form Fe 3O 4Particle.Oxidation style is with Fe 2+With oxygenant such as H 4N 2H 2The O partial oxygen changes into Fe 3+Form Fe 3O 4Particle.Reduction method is with Fe 3+With reductive agent such as Na 2SO 3Partial reduction becomes Fe 2+Three kinds of above methods can be synthesized the Z 250 particle in a large number, but shortcoming is to obtain monodispersed particle, and size distribution is wide, can not be scattered in again in the solvent behind the product drying, influences the superparamagnetism of particle, also is unfavorable for the application of particle.The organoiron compound thermal decomposition method is to allow organoiron compound such as ferric acetyl acetonade, iron carbonyl, iron oleates etc. carry out thermolysis in the high boiling organic solvent that has tensio-active agent to exist, obtain being connected to tensio-active agent can be in organic phase the Fe of good distribution 3O 4Particle.This method can obtain monodispersed Fe 3O 4Particle, but shortcoming is that most of organoiron compound toxicity is big, costs an arm and a leg, synthetic in enormous quantities cost height, and temperature of reaction generally needs 250 ℃～320 ℃ high temperature.
Publication number is that (application number: patent application 200510111014.1) discloses the method that a kind of preparation dissolves in the nano ferriferrous oxide of polar solvent to CN 1775694A, and this method is under the nitrogen protection condition, with FeCl 36H 2O and FeCl 24H 2The aqueous solution of O splashes in the mixing solutions of amine/non-polar solvent and reacts, take out reaction product after, adopt centrifugal method to obtain throw out, and, obtain nano ferriferrous oxide granule after the vacuum lyophilization with acetone and washed with de-ionized water.Though this method technical process is simple, sets up the continous way mode of production easily, the nano ferriferrous oxide granule size-grade distribution that is obtained is than homogeneous, and institute's nano ferriferrous oxide granule particle diameter that obtains is at 10nm～14nm, and can only be dissolved in the polar solvent.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of monodisperse, ultra paramagnetic ferroferric oxide (Fe that dissolves in non-polar solvent is provided 3O 4) nanometer particle process method, this kind method can not only obtain the nano ferriferrous oxide granule of particle diameter less than 10nm, and narrow diameter distribution, is typical monodisperse particle.
Monodisperse, ultra paramagnetic ferroferric oxide (Fe of the present invention 3O 4) nanometer particle process method, processing step is as follows:
(1) batching
Raw material comprises Fe 3+Soluble salt, Fe 2+Soluble salt, anion surfactant and mixed solvent, Fe 3+With Fe 2+The ratio of amount of substance is 2:1, anion surfactant and Fe 3+And Fe 2+The ratio of total amount of substance be 0.5～2:1,
Mixed solvent is by the organic solvent that dissolves each other with water, formulated with immiscible organic solvent of water and water, and the volume ratio of each component of mixed solvent is:
The organic solvent that dissolves each other with water: water=1～3:1,
The organic solvent and the water that dissolve each other with water: with the immiscible organic solvent=1:0.5 of water～2;
(2) mix and backflow
Under room temperature (indoor natural temperature), nitrogen protection with Fe 3+Soluble salt, Fe 2+Soluble salt, anion surfactant and mixed solvent are added in the container, and mix, treat that solid matter dissolves fully, water becomes colorless, when being brown with the immiscible organic phase-change of water, being heated to reflux temperature (reflux temperature is determined by mixed solvent) refluxes, return time 10min-4h promptly finishes reaction;
(3) cooling, separation, washing, drying
After stopping to reflux, be cooled to room temperature, add separating agent and make Fe 3O 4Particle is separated out, and adopts centrifugal separation with Fe then 3O 4Particle is separated from solvent, with behind the detergent washing in vacuum drying oven dry Nano particles of monodisperse, ultra paramagnetic ferroferric oxide.
For fast reaction speed, at Fe 3+Soluble salt, Fe 2+The mixed processes of soluble salt, anion surfactant and mixed solvent treats that solid matter dissolves fully, can add alkaline matter with the immiscible organic phase-change of water during for brown and stir, and institute adds alkaline matter and Fe 3+And Fe 2+The ratio of total amount of substance be 0.5～5:1.Alkaline matter comprises mineral alkali, organic bases, and mineral alkali is sodium hydroxide or potassium hydroxide or ammoniacal liquor, and organic bases is positive Tributylamine or pyridine.
In the aforesaid method, Fe 3+Soluble salt, Fe 2+Soluble salt is muriate or the vitriol of iron or the nitrate of iron of iron.
In the aforesaid method, anion surfactant is a kind of in sodium stearate, sodium oleate, sodium laurylsulfonate, the Sodium dodecylbenzene sulfonate.
In the aforesaid method, the organic solvent that dissolves each other with water is ethanol or methyl alcohol, with the immiscible organic solvent of water be toluene or dimethylbenzene or benzyl oxide or phenylate, 70～85 ℃ of reflux temperatures.
In the aforesaid method, separating agent is ethanol or methyl alcohol, and the consumption of separating agent is: the separating agent volume: with the immiscible organic solvent volume of water=1～2:1.Washing composition is normal hexane and ethanol or normal hexane and methyl alcohol, during washing, alternately washs 3～5 times with normal hexane and ethanol or normal hexane and methyl alcohol.
The present invention has following beneficial effect:
1, the Fe of the method for the invention preparation 3O 4The particle monodispersity is good, detects with the dynamic light scattering particle size instrument, and the granularity peak concentrates on 4～7nm, and peak width has only about 1.5nm and (sees Fig. 3, Fig. 4).
2, the Fe of the method for the invention preparation 3O 4The particle diameter of particle is little, uses transmission electron microscope observation, and particle diameter only is 3 nanometers～4 nanometers (seeing Fig. 1, Fig. 2).
3, the Fe of the method for the invention preparation 3O 4Particle has good superparamagnetism energy, and saturation magnetization Ms is not less than 15emu/g, and coercive force is 0Oe (seeing Fig. 5, Fig. 6); Tb is about 25K, and illustrative material is superparamagnetism (seeing Fig. 7, Fig. 8) when being higher than 25K.
4, can preserve by solid form after the ferriferrous oxide nano-particle drying of the method for the invention preparation, can be scattered in again in the non-polar organic solvent during use, size and distribution are all unaffected.
5, by adding tensio-active agent (hexadecyl brometo de amonio etc.), can forward the ferriferrous oxide nano-particle of the preparation of dispersive the method for the invention in organic phase to aqueous phase, become water-soluble divided particles, in aqueous environments, use.
6, raw material is the chemical product that routinizes, originate wide, cheap, nontoxic, cost is low.
7, the preparation method is simple, and a step finishes, and temperature of reaction is lower than 100 ℃.
Description of drawings
Fig. 1, Fig. 2 are the transmission electron microscope photos of the ferriferrous oxide nano-particle that dissolves in non-polar solvent of the method for the invention preparation;
Fig. 3, Fig. 4 are the particle size distribution figures of the ferriferrous oxide nano-particle that dissolves in non-polar solvent of the method for the invention preparation, record with the dynamic light scattering particle size instrument;
Fig. 5, Fig. 6 are the magnetic hysteresis loop figure of the ferriferrous oxide nano-particle that dissolves in non-polar solvent of the method for the invention preparation;
Fig. 7, Fig. 8 are the M-T curves of the ferriferrous oxide nano-particle that dissolves in non-polar solvent of the method for the invention preparation.
Embodiment
Embodiment 1
The processing step of present embodiment is as follows:
(1) batching
Fe 3+Soluble salt is 3.60g FeCl 36H 2O, Fe 2+Soluble salt is 1.33g FeCl 24H 2O, anion surfactant are 16.21g sodium oleate (C 18H 33ONa), mixed solvent is formulated by 30ml water, 40ml ethanol and 70ml toluene;
(2) mix and backflow
Under room temperature (16 ℃), nitrogen protection, mixed solvent is added in the flask, then with FeCl 36H 2O, FeCl 24H 2O and sodium oleate (C 18H 33ONa) add in the flask, and mix, treat that solid matter in the flask dissolves fully and water-fast toluene color transition when being brown, place oil bath to be heated to 74 ℃ of reflux temperatures, backflow 4h in flask;
(3) cooling, separation, washing, drying
After stopping to reflux, be cooled to room temperature, add 70ml ethanol (separating agent), make Fe 3O 4Particle is separated out, and centrifugal then 1 minute (4000 rev/mins) are with Fe 3O 4Particle is separated from solvent, alternately washs 3 times with washing composition normal hexane and ethanol, and washing back dry 8h in vacuum drying oven gets monodisperse, ultra paramagnetic Fe 3O 4Nanoparticle, drying temperature are 60 ℃, and vacuum tightness is 0.095KPa.
Embodiment 2
The processing step of present embodiment is as follows:
(1) batching
Fe 3+Soluble salt is 3.60g FeCl 36H 2O, Fe 2+Soluble salt is 1.33g FeCl 24H 2O, anion surfactant are 16.21g sodium oleate (C 18H 33ONa), alkaline matter is 0.8g NaOH, and mixed solvent is formulated by 40ml water, 40ml ethanol and 40ml toluene;
(2) mix and backflow
Under room temperature (20 ℃), nitrogen protection, mixed solvent is added in the flask, then with FeCl 36H 2O, FeCl 24H 2O and C 18H 33ONa adds in the flask, and mixes, and treats that solid matter in the flask dissolves fully and water-fast toluene color transition when being brown, adds NaOH and stirs, and then flask is placed oil bath to be heated to 74 ℃ of reflux temperatures, backflow 2h;
(3) cooling, separation, washing, drying
After stopping to reflux, be cooled to room temperature, add 70ml methyl alcohol (separating agent), make Fe 3O 4Particle is separated out, and centrifugal then 1 minute (4000 rev/mins) are with Fe 3O 4Particle is separated from solvent, alternately washs 3 times with washing composition normal hexane and methyl alcohol, and washing back dry 12h in vacuum drying oven, drying temperature is 40 ℃, vacuum tightness is 0.095KPa.Gained monodisperse, ultra paramagnetic Fe 3O 4The nano particle diameter size is 3～4nm (see figure 1), and the granularity peak concentrates on 6.36nm, peak width 1.53nm (see figure 3), magnetic saturation intensity is 20.3emu/g, coercive force is the 0Oe (see figure 5), and the Tb temperature is 24.5K, and illustrative material is super paramagnetic (see figure 7) when being higher than 24.5K.
Embodiment 3
The processing step of present embodiment is as follows:
(1) batching
Fe 3+Soluble salt is 5.39g Fe (NO 3) 39H 2O, Fe 2+Soluble salt is 1.20g Fe (NO 3) 2, anion surfactant is 32.62g sodium stearate (C 17H 35COONa), alkaline matter is 0.22g KOH, and mixed solvent is formulated by 30ml water, 60ml ethanol and 90ml dimethylbenzene;
(2) mix and backflow
Under room temperature (5 ℃), nitrogen protection, mixed solvent is added in the flask, then with Fe (NO 3) 39H 2O, Fe (NO 3) 2And C 17H 35COONa adds in the flask, and mix, treat that solid matter in the flask dissolves fully and water-fast dimethylbenzene color transition when being brown, add KOH and stir, then flask is placed oil bath to be heated to 80 ℃ of reflux temperatures, backflow 30min;
(3) cooling, separation, washing, drying
After stopping to reflux, be cooled to room temperature, add 180ml ethanol (separating agent), make Fe 3O 4Particle is separated out, and centrifugal then 2 minutes (3500 rev/mins) are with Fe 3O 4Particle is separated from solvent, alternately washs 5 times with washing composition normal hexane and ethanol, and washing back dry 16h in vacuum drying oven gets monodisperse, ultra paramagnetic Fe 3O 4Nanoparticle, drying temperature are 20 ℃, and vacuum tightness is 0.095KPa.
Embodiment 4
The processing step of present embodiment is as follows:
(1) batching
Fe 3+Soluble salt is 5.33g Fe 2(SO 4) 3, Fe 2+Soluble salt is 0.99g FeSO 4, anion surfactant is 14.50g sodium laurylsulfonate (C 12H 25SO 3Na), alkaline matter is the dense NH of 0.77ml 3H 2O, mixed solvent is formulated by 40ml water, 40ml ethanol and 160ml benzyl oxide;
(2) mix and backflow
Under room temperature (10 ℃), nitrogen protection, mixed solvent is added in the flask, then with Fe (NO 3) 39H 2O, Fe (NO 3) 2And C 12H 25SO 3Na adds in the flask, and mixes, and treats that solid matter in the flask dissolves fully and water-fast benzyl oxide color transition when being brown, adds ammoniacal liquor and stirs, and then flask is placed oil bath to be heated to 83 ℃ of reflux temperatures, backflow 10min;
(3) cooling, separation, washing, drying
After stopping to reflux, be cooled to room temperature, add 160ml methyl alcohol (separating agent), make Fe 3O 4Particle is separated out, and centrifugal then 3 minutes (3000 rev/mins) are with Fe 3O 4Particle is separated from solvent, alternately washs 3 times with washing composition normal hexane and methyl alcohol, and washing back dry 24h in vacuum drying oven gets monodisperse, ultra paramagnetic Fe 3O 4Nanoparticle, drying temperature are 20 ℃, and vacuum tightness is 0.095KPa.
Embodiment 5
The processing step of present embodiment is as follows:
(1) batching
Fe 3+Soluble salt is 1.8g FeCl 36H 2O, Fe 2+Soluble salt is 0.66g FeCl 24H 2O, anion surfactant are 9.28g Sodium dodecylbenzene sulfonate (C 18H 29SO 3Na), alkaline matter is 0.4g NaOH, and mixed solvent is formulated by 15ml water, 20ml methyl alcohol and 18ml phenylate;
(2) mix and backflow
Under room temperature (15 ℃), nitrogen protection, mixed solvent is added in the flask, then with FeCl 36H 2O, FeCl 24H 2O and C 18H 29SO 3Na adds in the flask, and mixes, and treats that solid matter in the flask dissolves fully and water-fast phenylate color transition when being brown, adds NaOH and stirs, and then flask is placed oil bath to be heated to 82 ℃ of reflux temperatures, backflow 3h;
(3) cooling, separation, washing, drying
After stopping to reflux, be cooled to room temperature, add 18ml ethanol (separating agent), make Fe 3O 4Particle is separated out, and centrifugal then 1 minute (4000 rev/mins) are with Fe 3O 4Particle is separated from solvent, alternately washs 4 times with washing composition normal hexane and ethanol, and washing back dry 8h in vacuum drying oven gets monodisperse, ultra paramagnetic Fe 3O 4Nanoparticle, drying temperature are 60 ℃, and vacuum tightness is 0.095KPa.
Embodiment 6
The processing step of present embodiment is as follows:
(1) batching
Fe 3+Soluble salt is 1.8g FeCl 36H 2O, Fe 2+Soluble salt is 0.66g FeCl 24H 2O, anion surfactant are 4.06g sodium oleate (C 18H 33ONa), alkaline matter is positive the Tributylamine ((C of 15mL 4H 9) 3N), mixed solvent is formulated by 15ml water, 45ml ethanol and 60ml toluene;
(2) mix and backflow
Under room temperature (25 ℃), nitrogen protection, mixed solvent is added in the flask, then with FeCl 36H 2O, FeCl 24H 2O and C 18H 33ONa adds in the flask, and mixes, and treats that solid matter in the flask dissolves fully and water-fast toluene color transition when being brown, adds (C 4H 9) 3N stirs, and then flask is placed oil bath to be heated to 74 ℃ of reflux temperatures, backflow 1h;
(3) cooling, separation, washing, drying
After stopping to reflux, be cooled to room temperature, add 90ml ethanol (separating agent), make Fe 3O 4Particle is separated out, and centrifugal then 1 minute (4000 rev/mins) are with Fe 3O 4Particle is separated from solvent, alternately washs 3 times with washing composition normal hexane and ethanol, and washing back dry 8h in vacuum drying oven gets monodisperse, ultra paramagnetic Fe 3O 4Nanoparticle, drying temperature are 60 ℃, and vacuum tightness is 0.095KPa.
Embodiment 7
The processing step of present embodiment is as follows:
(1) batching
Fe 3+Soluble salt is 1.8g FeCl 36H 2O, Fe 2+Soluble salt is 0.66g FeCl 24H 2O, anion surfactant are 8.11g sodium oleate (C 18H 33ONa), alkaline matter is 3.48ml pyridine (C 5H 5N), mixed solvent is formulated by 20ml water, 20ml ethanol and 40ml toluene;
(2) mix and backflow
Under room temperature (30 ℃), nitrogen protection, mixed solvent is added in the flask, then with FeCl 36H 2O, FeCl 24H 2O and C 18H 33ONa adds in the flask, and mixes, and treats that solid matter in the flask dissolves fully and water-fast toluene color transition when being brown, adds C 5H 5N stirs, and then flask is placed oil bath to be heated to 74 ℃ of reflux temperatures, backflow 4h;
(3) cooling, separation, washing, drying
After stopping to reflux, be cooled to room temperature, add 40ml ethanol (separating agent), make Fe 3O 4Particle is separated out, and centrifugal then 1 minute (4000 rev/mins) are with Fe 3O 4Particle is separated from solvent, alternately washs 3 times with washing composition normal hexane and ethanol, and washing back dry 16h in vacuum drying oven, drying temperature is 20 ℃, vacuum tightness is 0.095KPa.
Gained monodisperse, ultra paramagnetic Fe 3O 4The nano particle diameter size is 3～4nm (see figure 2), and the granularity peak concentrates on 6.43nm, peak width 1.59nm (see figure 4), and magnetic saturation intensity is 15.1emu/g, and coercive force is the 0Oe (see figure 6), and the Tb temperature is 25.0K, is super paramagnetic (see figure 8) at normal temperatures.
The monodisperse, ultra paramagnetic Fe of embodiment 1, embodiment 3, embodiment 4, embodiment 5 and embodiment 6 preparations 3O 4The nano particle diameter size is 3～4nm, and the granularity peak concentrates on 4～7nm, and about peak width 1.5nm, magnetic saturation intensity is not less than 15emu/g, and coercive force is 0Oe, and the Tb temperature is about 25.0K, and illustrative material is super paramagnetic when being higher than 25.0K.

Claims (10)

1, a kind of preparation method of Nano particles of monodisperse, ultra paramagnetic ferroferric oxide is characterized in that processing step is as follows:
(1) batching
Raw material comprises Fe 3+Soluble salt, Fe 2+Soluble salt, anion surfactant and mixed solvent, Fe 3+With Fe 2+The ratio of amount of substance is 2: 1, anion surfactant and Fe 3+And Fe 2+The ratio of total amount of substance be 0.5～2: 1,
Mixed solvent is by the organic solvent that dissolves each other with water, formulated with immiscible organic solvent of water and water, and the volume ratio of each component of mixed solvent is:
The organic solvent that dissolves each other with water: water=1～3: 1,
The organic solvent and the water that dissolve each other with water: with the immiscible organic solvent of water=1: 0.5～2;
(2) mix and backflow
Under room temperature, nitrogen protection with mixed solvent, Fe 3+Soluble salt, Fe 2+Soluble salt and anion surfactant add in the reaction vessel, and mix, and treat that solid matter dissolves fully, when being brown with the immiscible organic phase-change of water, being heated to reflux temperature and refluxing, and return time 10min-4h promptly finishes reaction;
(3) cooling, separation, washing, drying
After stopping to reflux, be cooled to room temperature, add separating agent ethanol or methyl alcohol the Fe3O4 particle is separated out, adopt centrifugal separation then Fe 3O 4Particle is separated from solvent, with behind the detergent washing in vacuum drying oven dry Nano particles of monodisperse, ultra paramagnetic ferroferric oxide.
2, the preparation method of Nano particles of monodisperse, ultra paramagnetic ferroferric oxide according to claim 1 is characterized in that raw material also comprises alkaline matter, alkaline matter and Fe 3+And Fe 2+The ratio of total amount of substance be 0.5～5: 1,
At Fe 3+Soluble salt, Fe 2+The mixed processes of soluble salt, anion surfactant and mixed solvent treats that solid matter dissolves fully, adds alkaline matter with the immiscible organic phase-change of water during for brown and stir.
3, the preparation method of Nano particles of monodisperse, ultra paramagnetic ferroferric oxide according to claim 2 is characterized in that alkaline matter is a kind of in sodium hydroxide, potassium hydroxide, ammoniacal liquor, positive Tributylamine, the pyridine.
4, according to the preparation method of claim 1 or 2 or 3 described Nano particles of monodisperse, ultra paramagnetic ferroferric oxide, it is characterized in that Fe 3+Soluble salt, Fe 2+Soluble salt is muriate or the vitriol of iron or the nitrate of iron of iron.
5,, it is characterized in that anion surfactant is a kind of in sodium stearate, sodium oleate, sodium laurylsulfonate, the Sodium dodecylbenzene sulfonate according to the preparation method of claim 1 or 2 or 3 described Nano particles of monodisperse, ultra paramagnetic ferroferric oxide.
6, according to the preparation method of claim 1 or 2 or 3 described Nano particles of monodisperse, ultra paramagnetic ferroferric oxide, it is characterized in that in the mixed solvent, the organic solvent that dissolves each other with water is ethanol or methyl alcohol, with the immiscible organic solvent of water be toluene or dimethylbenzene or benzyl oxide or phenylate.
7, the preparation method of Nano particles of monodisperse, ultra paramagnetic ferroferric oxide according to claim 5 is characterized in that reflux temperature is 70～85 ℃.
8, the preparation method of Nano particles of monodisperse, ultra paramagnetic ferroferric oxide according to claim 6 is characterized in that reflux temperature is 70～85 ℃.
9, according to the preparation method of claim 1 or 2 or 3 described Nano particles of monodisperse, ultra paramagnetic ferroferric oxide, it is characterized in that the consumption of separating agent ethanol or methyl alcohol is: the separating agent volume: with the immiscible organic solvent volume of water=1～2: 1.
10, according to the preparation method of claim 1 or 2 or 3 described Nano particles of monodisperse, ultra paramagnetic ferroferric oxide, it is characterized in that washing composition is normal hexane and ethanol or normal hexane and methyl alcohol, during washing, alternately wash 3～5 times with normal hexane and ethanol or normal hexane and methyl alcohol.
CNB2007100482663A 2007-01-15 2007-01-15 Method for preparing Nano particles of monodisperse, ultra paramagnetic ferroferric oxide Expired - Fee Related CN100522824C (en)

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