CN101759145A - Preparation method of ZnO/TiO2 composite nanoparticles - Google Patents

Abstract

The present invention discloses a preparation method of ZnO/TiO2 composite nanoparticles, which comprises the following steps: 1) ZnSO4 7H2O and NaCl or KCL according to the mole ratio of 1:5 to 1:15 are mixed evenly at room temperature, and are lapped for 5 min to 15 min into a white paste form; 2) NaOH or KOH is added according to the mole ratio of ZnSO4 7H2O and NaOH or KOH of 1:2 to 1:3 to be continually lapped 15 min to 25 min at the room temperature into light yellow powder; 3) tetrabutyl titanate is added according to the mole ratio of ZnSO4 7H2O and tetrabutyl titanate of 1:1 to 1:0.1 to be mixed evenly into paste, and is lapped continuously for 10min to 20 min to obtain white solid thin powder; the white solid thin powder is stirred and mixed by twice water, and is processed by supersound for 8min to 10min to be centrifuged and separated until chloride ions can not be detected in supernatant liquor; and the separated products are placed in a vacuum drying chamber to be dried for a plurality of hours under 75 DEG C, and then, the ZnO/TiO2 composite nanoparticles are obtained. The ZnO/TiO2 composite nanoparticles have good infrared absorptive performance, and has huge application prospect in the application of photocatalysis, photodegradation and the like.

Description

A kind of ZnO/TiO 2The preparation method of composite nanoparticle

Technical field

The present invention relates to a kind of ZnO/TiO ₂The preparation method of composite nanoparticle.

Background technology

In numerous nano-metal-oxides, ZnO has the band gap (3.37eV) of broad and higher exciton binding energy (60meV) as important II-VI family semi-conducting material, and nontoxic, cheap, environmental stability is good, exactly because these excellent performances of zinc oxide, the ZnO nano semiconductor material has been widely used in every field: electrooptical device, sensor, photovoltaic material, piezoelectric, cell marking, protein detection, ultraviolet light detection etc.At present, the main synthetic method of ZnO nano material has: microwave method, sol-gal process, hydro-thermal method, coprecipitation, solution calcination method, thermal decomposition method, gas-phase condensation method, thermal evaporation, direct polishing and chemical mechanical pulping or the like. but all in liquid phase, finish mostly in the above cited method, however solid phase is synthetic relatively, and liquid phase is synthesized the weak point that itself is arranged, such as: the nucleating growth process has notable difference and some reaction speed is too fast, process is difficult to control, and the trickle change on the dynamics will cause structure, modal great variety.

Summary of the invention

The purpose of this invention is to provide a kind of ZnO/TiO ₂The preparation method of composite nanoparticle.

The objective of the invention is to realize in the following way: 1, a kind of ZnO/TiO ₂The preparation method of composite nanoparticle: it is characterized in that:

1), presses ZnSO ₄7H ₂The mol ratio of O and NaCl or KCl is: at room temperature mixed in 1: 5～1: 15, and ground 5-10min, become white paste form;

2), press ZnSO ₄7H ₂The mol ratio of O and NaOH or KOH is: 1: 2～1: 3, add NaOH or KOH, and continue to grind 15-25min under the room temperature, form flaxen fine powder;

3), press ZnSO ₄7H ₂The mol ratio of O and tetra-n-butyl titanate is: 1: 1～1: 0.1, add tetra-n-butyl titanate, and be mixed into paste, and continue to grind 10-20min, obtain the pressed powder of white; The pressed powder that will arrive white mixes with secondary water, and ultrasonic 8-10min, and centrifugation can not detect chlorion and exists in supernatant liquor, separated product is placed vacuum drying chamber, 75 ℃ of down dry a few hours, has promptly obtained ZnO/TiO ₂Composite nanoparticle.

The present invention has following beneficial effect: 1, technological process is simple, and the reaction time is short, and is with low cost; 2, whole process of preparation need not any organic solvent, and reaction temperature only needs room temperature to get final product, and need not last handling processes such as high annealing; 3, the advantage in the reactive matrix system continues as next step doping system service, form the compound system 4 of two kinds of nano particles, prepared composite nanoparticle particle diameter comparatively meticulous (3～20nm), favorable dispersibility, be dispersed in the organic solvent such as methyl alcohol and do not see a sedimentation yet in month, reunite; 5, by regulating ZnSO in the compound system ₄7H ₂The mol ratio that O is different with tetra-n-butyl titanate is (1: 1～1: 0.1), and its performance can obtain raising in various degree; 6, composite nanoparticle significantly strengthens UV Absorption, can be used for photocatalysis, light degradation etc.;

The specific embodiment

Below in conjunction with embodiment the present invention is described in further detail.

Embodiment 1

At first, with the ZnSO of 1.0g ₄7H ₂The NaCl of O and 2.5g at room temperature mixes, and grinds 10min, becomes white paste form.Then, the NaOH powder of 0.28g is joined in the above mixed system, continue to grind 20min under the room temperature, form flaxen fine powder.At last, accurately pipette 1.19ml tetra-n-butyl titanate (ZnSO with pipette ₄7H ₂The mol ratio of O and tetra-n-butyl titanate is: 1: 1) join in the above mixed-powder, be mixed into paste, and continue to grind 10-20min, obtain the pressed powder of white.End product is mixed with secondary water, and ultrasonic 8-10min, centrifugation repeats for several times, can not detect chlorion and exist in supernatant liquor, and separated product is placed vacuum drying chamber, 75 ℃ of down dry a few hours, has promptly obtained ZnO and TiO ₂Composite nanoparticle.

Embodiment 2

Take by weighing the ZnSO of 1.0g ₄7H ₂The KCl of O and 3.0g mixes, griding reaction 10min.Then, take by weighing the KOH of 0.39g and join in the above mixed-powder, mix, continue griding reaction 20min, form the fine powder of little Huang.At last, accurately pipette tetra-n-butyl titanate 1.19ml (ZnSO with pipette ₄7H ₂The mol ratio of O and tetra-n-butyl titanate is: 1: 1) add wherein, griding reaction is complete to the tetra-n-butyl titanate hydrolysis, forms meticulous white powder.With product for several times with the ultrasonic cleaning of secondary water, no chlorion existence in centrifugal clear liquid, 70 ℃ of vacuum drying 5 hours obtain ZnO and TiO ₂Composite nanoparticle.

Embodiment 3

Take by weighing the ZnSO of 1.0g ₄7H ₂The KCl of O and 3.0g mixes, griding reaction 10min.Then, take by weighing the KOH of 0.39g and join in the above mixed-powder, mix, continue griding reaction 20min, form the fine powder of little Huang.At last, accurately pipette tetra-n-butyl titanate 0.60ml (ZnSO with pipette ₄7H ₂The mol ratio of O and tetra-n-butyl titanate is: 1: 0.3) add wherein, griding reaction is complete to the tetra-n-butyl titanate hydrolysis, forms meticulous white powder.With product for several times with the ultrasonic cleaning of secondary water, no chlorion existence in centrifugal clear liquid, 70 ℃ of vacuum drying 5 hours obtain ZnO and TiO ₂Composite nanoparticle.

Embodiment 4

Take by weighing the ZnSO of 1.0g ₄7H ₂The KCl of O and 3.0g mixes, griding reaction 10min.Then, take by weighing the KOH of 0.39g and join in the above mixed-powder, mix, continue griding reaction 20min, form the fine powder of little Huang.At last, accurately pipette tetra-n-butyl titanate 0.30ml (ZnSO with pipette ₄7H ₂The mol ratio of O and tetra-n-butyl titanate is: 1: 0.2) add wherein, griding reaction is complete to the tetra-n-butyl titanate hydrolysis, forms meticulous white powder.With product for several times with the ultrasonic cleaning of secondary water, no chlorion existence in centrifugal clear liquid, 70 ℃ of vacuum drying 5 hours obtain ZnO and TiO ₂Composite nanoparticle.

Embodiment 5

Take by weighing the ZnSO of 1.0g ₄7H ₂The KCl of O and 3.0g mixes, griding reaction 10min.Then, take by weighing the KOH of 0.39g and join in the above mixed-powder, mix, continue griding reaction 20min, form the fine powder of little Huang.At last, accurately pipette tetra-n-butyl titanate 0.12ml (ZnSO with pipette ₄7H ₂The mol ratio of O and tetra-n-butyl titanate is: 1: 0.1) add wherein, griding reaction is complete to the tetra-n-butyl titanate hydrolysis, forms meticulous white powder.With product for several times with the ultrasonic cleaning of secondary water, no chlorion existence in centrifugal clear liquid, 70 ℃ of vacuum drying 5 hours obtain ZnO and TiO ₂Composite nanoparticle.

Claims (1)

1. ZnO/TiO ₂The preparation method of composite nanoparticle: it is characterized in that:

1), presses ZnSO ₄7H ₂The mol ratio of O and NaCl or KCl is: at room temperature mixed in 1: 5～1: 15, and ground 5-10min, become white paste form;

2), press ZnSO ₄7H ₂The mol ratio of O and NaOH or KOH is: 1: 2～1: 3, add NaOH or KOH, and continue to grind 15-25min under the room temperature, form flaxen fine powder;

3), press ZnSO ₄7H ₂The mol ratio of O and tetra-n-butyl titanate is: 1: 1～1: 0.1, add tetra-n-butyl titanate, and be mixed into paste, and continue to grind 10-20min, obtain the pressed powder of white; The pressed powder that will arrive white mixes with secondary water, and ultrasonic 8-10min, and centrifugation can not detect chlorion and exists in supernatant liquor, separated product is placed vacuum drying chamber, 75 ℃ of down dry a few hours, has promptly obtained ZnO/TiO ₂Composite nanoparticle.