CN100431969C - Preparation method of nano-metal oxide - Google Patents

Preparation method of nano-metal oxide Download PDF

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Publication number
CN100431969C
CN100431969C CNB2006101316115A CN200610131611A CN100431969C CN 100431969 C CN100431969 C CN 100431969C CN B2006101316115 A CNB2006101316115 A CN B2006101316115A CN 200610131611 A CN200610131611 A CN 200610131611A CN 100431969 C CN100431969 C CN 100431969C
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nitrate
metal
nano
grain
size
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CN1948158A (en
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李德谦
张绘
孟淑兰
李红飞
张志峰
国富强
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Changzhou Institute Of Energy Storage Materials & Devices
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Changchun Institute of Applied Chemistry of CAS
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Abstract

The present invention belongs to a preparation method of nano metal oxide. It is characterized by that said invention makes the metal nitrate be thermally-decomposed in the range of 300 deg.C-900 deg.C, heating time is 10 min-120 min, so as to obtain the nano metal oxide. The described metal nitrate is the nitrate of La,Ce,Pr,Nd,Pm, Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,Y,Sc,and Zr.

Description

A kind of preparation method of nano-metal-oxide
Technical field
The invention belongs to a kind of preparation method of nano-metal-oxide.
Background technology
Metal oxide has purposes widely in industrial application, catalyzer for example, optical material, burnishing agent or the like.The preparation method of nano-metal-oxide generally comprises microemulsion method, hydrothermal method, hydrolysis method, the precipitator method, thermal decomposition method etc.For example Chinese patent CN1136016A adopts a kind of improved rare-earth oxalate thermolysis process to prepare the rare earth oxide of large specific surface; Chinese patent CN1389403A adopts ammonium bicarbonate precipitation rare earth soluble salt, adds tensio-active agent then in the filter cake and stirs, and drying then, calcining method prepares oxide nano rare earth.
It is precipitation agent that Chinese patent 93103702.6 discloses with carbonate or carbonic acid gas, and precipitating rare earth nitrate or chloride soln form Re 2(CO 3) 3Precipitation, filtering drying keeps constant temperature to make carbonate decomposition, and slowly is converted into oxide compound, is warming up to 850 ℃ then, makes the ultra micro RE oxide powder.Is 40nm～50nm by tem observation to particle diameter.
Chinese patent application number 01108144.9 discloses and has added basic solution in the rare-earth chloride solution, produces precipitation, and throw out is carried out drying, washing, add alcohols material then, mix, thermal degradation, crushing screening makes the rare earth oxide that grain-size is 22nm～50nm.
It is many that the preparation method of present metal oxide, especially preparation of nanomaterials all exist preparation process, cost height, the problem that granularity is bigger.
Summary of the invention
In order to address these problems, the contriver adopts metal nitrate pyrolysated method to prepare nano-metal-oxide.For realizing above-mentioned purpose, the technical solution used in the present invention is: make metal nitrate thermolysis in 300 ℃～900 ℃ temperature ranges, be 10min～120min heat-up time, prepares metal oxide; Described metal nitrate comprises: described metal nitrate is: the nitrate of La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, Sc or Zr; This metal nitrate and NH 4NO 3The double salt that forms; This metal nitrate and NH 4NO 3The mixture that forms; The mixture that this metal nitrate is formed; Or this metal nitrate, metal nitrate and NH 4NO 3The mixture that the double salt that forms forms with arbitrary proportion again.
Beneficial effect of the present invention: the metal oxide grain-size that the present invention prepares is 5nm～25nm.The invention is characterized in that the nano-metal-oxide of preparing can be the oxide compound of single metallic element, also can be the mixed oxide of multiple metallic element.Method simple and fast of the present invention can obtain the nanoparticle of reduced size.
Embodiment:
Embodiment 1
Get 1g Pr (NO 3) 3Solid with 500 ℃ of temperature heating 30min, obtains black powder in retort furnace, XRD turns out to be Pr 6O 11, and to calculate its grain-size by the Scherrer formula be 11.2nm.
Embodiment 2 3
Get 1gGd (NO 3) 34H 2The O solid with 500 ℃ of temperature heating 30min, obtains white powder in retort furnace, turn out to be Gd by XRD 2O 3, and to calculate its grain-size by the Scherrer formula be 12.7nm.
Embodiment 3 4
Get 1g Dy (NO 3) 34H 2The O solid with 500 ℃ of temperature heating 30min, obtains white powder in retort furnace, turn out to be Dy by XRD 2O 3, and to calculate its grain-size by the Scherrer formula be 11.5nm.
Embodiment 4
Get 1g Er (NO 3) 34H 2The O solid with 500 ℃ of temperature heating 30min, obtains pink powder in retort furnace, turn out to be Er by XRD 2O 3, and to calculate its grain-size by the Scherrer formula be 19.8nm.
Embodiment 5
Get 1g Yb (NO 3) 34H 2The O solid with 500 ℃ of temperature heating 30min, obtains white powder in retort furnace, turn out to be Yb by XRD 2O 3, and to calculate its grain-size by the Scherrer formula be 14.4nm.
Embodiment 6
Get 1g Y (NO 3) 36H 2The O solid with 500 ℃ of temperature heating 30min, obtains white powder in retort furnace, turn out to be Y by XRD 2O 3, and to calculate its grain-size by the Scherrer formula be 8.5nm.
Embodiment 7
Get 1g Zr (NO 3) 46H 2The O solid with 600 ℃ of temperature heating 30min, obtains white powder in retort furnace, turn out to be ZrO by XRD 2, and to calculate its grain-size by the Scherrer formula be 11.4nm.
Embodiment 8
Get 1g La (NO 3) 36H 2The O solid with 900 ℃ of temperature heating 30min, obtains white powder in retort furnace, turn out to be La by XRD (X-ray diffraction) 2O 3, and to calculate its grain-size by the Scherrer formula be 25nm.
Embodiment 9
Get 1g Ce (NO 3) 36H 2The O solid with 500 ℃ of temperature heating 30min, obtains pale yellow powder in retort furnace, turn out to be CeO by XRD 2, and to calculate its grain-size by the Scherrer formula be 10.3nm.
Embodiment 10
Get 1g (NH 4) 2Ce (NO 3) 6, in retort furnace,, obtain pale yellow powder with 300 ℃ of temperature heating 2h, turn out to be CeO by XRD 2, and to calculate its grain-size by the Scherrer formula be 3nm.
Embodiment 11
Get 1g (NH 4) 2Ce (NO 3) 6Solid with 500 ℃ of temperature heating 30min, obtains pale yellow powder in retort furnace, turn out to be CeO by XRD 2, and to calculate its grain-size by the Scherrer formula be 6.4nm.
Embodiment 12
Get 1g (NH 4) 2Ce (NO 3) 6, in retort furnace,, obtain pale yellow powder with 900 ℃ of temperature heating 10min, turn out to be CeO by XRD 2, and to calculate its grain-size by the Scherrer formula be 11.5nm.
Embodiment 13 2
Get 1g Ce (NO 3) 36H 2O and 5g NH 4NO 3Mix, in retort furnace,, obtain pale yellow powder, turn out to be CeO by XRD with 500 ℃ of temperature heating 30min 2, and to calculate its grain-size by the Scherrer formula be 9.5nm.
Embodiment 14
Get 1g (NH 4) 2Er (NO 3) 5Solid with 500 ℃ of temperature heating 30min, obtains pink powder in retort furnace, turn out to be Er by XRD 2O 3, and to calculate its grain-size by the Scherrer formula be 17.5nm.
Embodiment 15 3
Get 1g La (NO 3) 36H 2O and 2g NH 4NO 3Mix, in retort furnace,, obtain white powder, turn out to be La by XRD with 900 ℃ of temperature heating 30min 2O 3, and to calculate its grain-size by the Scherrer formula be 19.8nm.
Embodiment 16 4
Get 1g Yb (NO 3) 34H 2O and 0.02g (NH 4) 2Ce (NO 3) 6Mix, in retort furnace,, obtain white powder, turn out to be CeO by XRD with 500 ℃ of temperature heating 30min 2And La 2O 3, and to calculate its grain-size by the Scherrer formula be 5.5nm (CeO 2) and 13.1nm (Yb 2O 3).
Embodiment 17
Get 1g Zr (NO 3) 46H 2O and 1g (NH 4) 2Ce (NO 3) 6Mix, in retort furnace,, obtain pale yellow powder, turn out to be ZrO by XRD with 700 ℃ of temperature heating 30min 2And CeO 2, and to calculate its grain-size by the Scherrer formula be 11.9nm (ZrO 2) and 7.1nm (CeO 2).
Embodiment 18
Get 1g La (NO 3) 36H 2O and 0.02g Nd (NO 3) 36H 2O mixes, and with 900 ℃ of temperature heating 60min, obtains light blue powder in retort furnace, turns out to be La by XRD 2O 3/ Nd 2O 3, and to calculate its grain-size by the Scherrer formula be 22.5nm (La 2O 3) and 19.1nm (Nd 2O 3).
Embodiment 19
Get 1g Er (NO 3) 3With 1g Y (NO 3) 3And 0.2g (NH 4) 2Ce (NO 3) 6Mix, in retort furnace,, obtain the light red powder, turn out to be CeO by XRD with 500 ℃ of temperature heating 30min 2/ ErYO 3, and to calculate its grain-size by the Scherrer formula be 11.4nm (CeO 2) and 15.6nm (ErYO 3).

Claims (3)

1, a kind of nano-metal-oxide preparation method is characterized in that, makes metal nitrate thermolysis in 300 ℃～900 ℃ temperature ranges, and be 10min～120min heat-up time, prepares metal oxide; Described metal nitrate is: the nitrate of La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, Sc or Zr; This metal nitrate and NH 4NO 3The double salt that forms; This metal nitrate and NH 4NO 3The mixture that forms; The mixture that this metal nitrate is formed; Or the mixture of this metal nitrate, metal nitrate and NH 4NO 3The mixture that the double salt that forms forms with arbitrary proportion again.
2, a kind of nano-metal-oxide preparation method as claimed in claim 1 is characterized in that described metal nitrate is: the nitrate of La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, Sc or Zr and NH 4NO 3The double salt or the mixture that form.
3, a kind of nano-metal-oxide preparation method as claimed in claim 1, it is characterized in that described metal nitrate is: the mixture of the nitrate of La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, Sc or Zr, metal nitrate and NH 4NO 3The mixture that the double salt that forms forms with arbitrary proportion again.
CNB2006101316115A 2006-11-09 2006-11-09 Preparation method of nano-metal oxide Expired - Fee Related CN100431969C (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85103081A (en) * 1983-11-25 1986-10-22 考姆海克斯 From the aqueous solution of the nitrate of metal or the method that solid mixture is produced mealy metallic oxide
US5162299A (en) * 1990-12-14 1992-11-10 Hughes Aircraft Company Preparation of superconducting oxide precursor materials by pyrolysis from concentrated nitric acid solution

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85103081A (en) * 1983-11-25 1986-10-22 考姆海克斯 From the aqueous solution of the nitrate of metal or the method that solid mixture is produced mealy metallic oxide
US5162299A (en) * 1990-12-14 1992-11-10 Hughes Aircraft Company Preparation of superconducting oxide precursor materials by pyrolysis from concentrated nitric acid solution

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
六水合硝酸镧和六水合硝酸铈的热分解. 吴淑荣，熊为淼，何明安，宋迪生，刘翊纶.西北大学学报，第22期. 1981 *

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