CN104030349A - Method for synthesizing cerium-doped stable tetragonal-phase zirconia nanopowder by sol-gel method - Google Patents
Method for synthesizing cerium-doped stable tetragonal-phase zirconia nanopowder by sol-gel method Download PDFInfo
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- CN104030349A CN104030349A CN201410265772.8A CN201410265772A CN104030349A CN 104030349 A CN104030349 A CN 104030349A CN 201410265772 A CN201410265772 A CN 201410265772A CN 104030349 A CN104030349 A CN 104030349A
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Abstract
The invention relates to a method for synthesizing cerium-doped stable tetragonal-phase zirconia nanopowder by a sol-gel method. The method comprises the following steps: 1) selecting a certain amount of zirconium sources, cerium sources, surfactants and complexing agents, and respectively dissolving in a mixed solvent of water and ethanol to obtain mixed liquids; 2) dropwise adding the mixed liquids of zirconium sources, cerium sources and surfactants to the complexing agent liquid, and sufficiently stirring to obtain a mixed liquid; 3) heating the mixed liquid in a water bath under the condition of stirring, wherein the temperature of the water bath is 90-95 DEG C; 4) placing the gel obtained by heating in the water bath into an oven and drying at 120 DEG C; and 5) pulverizing the dried gel and calcining at 700-800 DEG C for 2 hours to obtain the final product. The synthesis process of the product is simple, the product is spherical particles of which the diameter is 10-20nm and has the characteristics of narrow particle size distribution range, excellent performance and low production cost.
Description
Technical field
The present invention relates to the preparation of nm-class powder of zirconium oxide, particularly the processing method of the stable tetragonal phase zirconium oxide nano powder of the synthetic cerium doping of a kind of sol-gel processing.
Background technology
Zirconia ceramics is a kind of very important structure and functional materials, has excellent physics and chemistry performance, has important using value and application prospect widely in fields such as biomedicine, catalysis, sensing, solid electrolyte, high-temperature flame-proofs.In recent years, tetragonal phase zirconium oxide pottery is owing to having good mechanical property, chemical stability, physiologically acceptable performance, more and more be subject to numerous investigators' attention in the application in the field such as aspect dental prosthetic material and joint prosthesis, be called the focus of domestic and international research.
Under normal pressure, zirconia ceramics has 3 kinds of crystal formations: monoclinic phase (m phase), Tetragonal (t) and Emission in Cubic (c), three kinds of crystal formations can mutually be changed in different temperature ranges.Emission in Cubic is high-temperature stable phase, and Tetragonal can be regarded Emission in Cubic as and extend and the crystalline structure of distortion along c-axis, and monoclinic phase can be regarded Tetragonal as and form along angle of β deflection.Tetragonal is attended by 3 ~ 5% volumetric expansion, the i.e. martensitic transformation of zirconia ceramics to the transformation of monoclinic phase.Recently research shows, zirconia-based ceramics in lesser temps, wet environment when long-term use, while being subject to the erosion of body fluid in particular as oral cavity material and joint material, H
2o molecule can be by filling ZrO
2oxygen room, top layer and enter into ZrO
2in the lattice of top layer, the filling of water molecules causes zirconia crystal lattice to be shunk, thereby produce tensile stress at grain surface and destroyed Tetragonal, the generation that causes Tetragonal to change to monoclinic phase, Tetragonal (t phase) causes its mechanical property to worsen to the transformation of monoclinic phase (m phase), has seriously restricted the use of zirconia-based ceramics.The performance of zirconia ceramics and application depend primarily on the aspect such as pattern, granularity and phase phase composite of its powder, therefore the nm-class powder of zirconium oxide that, how to obtain the Tetragonal that purity is high, activity is high, particle diameter is little, particle size distribution is narrow and stable has great importance.
Summary of the invention
Technical problem to be solved by this invention is the processing method of the stable tetragonal phase zirconium oxide nano powder that the synthetic cerium doping of a kind of sol-gel processing is provided, the method technique is simple, easy to operate, the powder purity making is high, particle diameter is little, and size range narrowly distributing, the doping of cerium has feature and the structural improvement effect of phase for synthetic tetragonal phase zirconium oxide powder granule, makes the purposes of tetragonal phase zirconium oxide powder more extensive, and biological chemical performance is more excellent.
The present invention is for solving the problems of the technologies described above, and the technical scheme adopting is: the processing method of the stable tetragonal phase zirconium oxide nano powder of the synthetic cerium doping of sol-gel processing, comprises the following steps:
(1) under room temperature, getting He Shi source, soluble zirconium source is dissolved in mixed solvent, afterwards, in mixing solutions, add tensio-active agent again, after being fully uniformly mixed, making containing zirconium ion concentration is 0.425-0.475 mol/L, and cerium ion concentration is 0.025-0.075 mol/L, tensio-active agent mass concentration is 2 ~ 5% mixed solution A, for subsequent use;
(2) separately get a certain amount of mixed solvent, add wherein complexing agent, after fully stirring, dissolving, making containing complexing agent concentration is the mixing solutions B of 0.5-0.6 mol/L, for subsequent use;
(3) by volume umber is got respectively the mixing solutions B that mixed solution A that 1 part of step (1) makes and 1 part of step (2) make, under agitation condition, the mixed solution A obtaining is added dropwise in mixing solutions B with the speed of 2ml/min, after fully mixing, obtains mixing solutions;
(4), under agitation condition, it is 90 ~ 95 that the mixing solutions that step (3) is obtained is put into temperature
oin the water-bath of C, carry out heating in water bath 72 h, obtain gel;
(5) gel step (4) being obtained is put into 120-130
oin the loft drier of C, be dried 10-12 h, obtain solid xerogel;
(6), after solid xerogel step (5) being obtained grinds, transposition enters in muffle furnace, is warming up to 700 ~ 800 with certain temperature rise rate
o, 700 ~ 800
ounder C condition, calcine 2h, obtain the stable tetragonal phase zirconium oxide nano powder of cerium doping.
Zirconium source described in step 1) is ZrOCl
28H
2o, cerium source is Ce (NO
3)
36H
2o, tensio-active agent is PEG600.
In step (1) and step (2), described mixed solvent is that volume ratio is the deionized water of 3 ~ 4:1 and the mixed solution of dehydrated alcohol.
Step 2) described complexing agent is C
6h
8o
7h
2o.
Drying temperature described in step 5) is 120
oc, be 10 h time of drying.
Calcining temperature rise rate described in step 6) is 3
oc/min.
Beneficial effect:
(1), the processing method of the stable tetragonal phase zirconium oxide nano powder of the synthetic cerium doping of a kind of sol-gel processing provided by the invention, can make Average Particle Diameters is the class spherical zircite nano-powder particle of 10 ~ 20 nm, its principal crystalline phase is Tetragonal, product purity is high, particle diameter is little, size range narrow distribution, and synthetic product granular size is controlled, and biological chemical performance is more excellent.
(2), the processing method of the stable tetragonal phase zirconium oxide nano powder of the synthetic cerium doping of a kind of sol-gel processing provided by the invention, technique is simple, easy to operate, raw materials cost doping low and cerium has feature and the structural improvement effect of phase for synthetic tetragonal phase zirconium oxide powder granule, makes the purposes of tetragonal phase zirconium oxide powder more extensive.
Brief description of the drawings
Fig. 1 is the Ce that embodiment 1 obtains
0.84zr
0.16o
2the XRD figure of cubic phase nano powder;
Fig. 2 is the Ce that embodiment 1 obtains
0.84zr
0.16o
2the TEM figure of cubic phase nano powder;
Fig. 3 is the Ce that embodiment 3 obtains
0.9zr
0.1o
2the XRD figure of cubic phase nano powder.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with example, but content of the present invention is not only confined to the following examples.
The processing method of the stable tetragonal phase zirconium oxide nano powder of the synthetic cerium doping of sol-gel processing, comprises the following steps:
(1) under room temperature, getting He Shi source, soluble zirconium source is dissolved in mixed solvent, afterwards, in mixing solutions, add tensio-active agent again, after being fully uniformly mixed, making containing zirconium ion concentration is 0.425-0.475 mol/L, and cerium ion concentration is 0.025-0.075 mol/L, tensio-active agent mass concentration is the mixed solution A of 2 ~ 5wt%, for subsequent use;
(2) separately get a certain amount of mixed solvent, add wherein complexing agent, after fully stirring, dissolving, making containing complexing agent concentration is the mixing solutions B of 0.5-0.6 mol/L, for subsequent use;
(3) by volume umber is got respectively the mixing solutions B that mixed solution A that 1 part of step (1) makes and 1 part of step (2) make, under agitation condition, the mixed solution A obtaining is added dropwise in mixing solutions B with the speed of 2ml/min, after fully mixing, obtains mixing solutions;
(4), under agitation condition, it is 90 ~ 95 that the mixing solutions that step (3) is obtained is put into temperature
oin the water-bath of C, carry out heating in water bath 72 h, obtain gel;
(5) gel step (4) being obtained is put into 120-130
oin the loft drier of C, be dried 10-12 h, obtain solid xerogel;
(6), after solid xerogel step (5) being obtained grinds, transposition enters in muffle furnace, is warming up to 700 ~ 800 with certain temperature rise rate
o, 700 ~ 800
ounder C condition, calcine 2h, obtain the stable tetragonal phase zirconium oxide nano powder of cerium doping.
Zirconium source described in step 1) is ZrOCl
28H
2o, cerium source is Ce (NO
3)
36H
2o, tensio-active agent is PEG600.
In step (1) and step (2), described mixed solvent is that volume ratio is the deionized water of 3 ~ 4:1 and the mixed solution of dehydrated alcohol.
Step 2) described complexing agent is C
6h
8o
7h
2o.
Drying temperature described in step 5) is 120
oc, be 10 h time of drying.
Calcining temperature rise rate described in step 6) is 3
oc/min.
Embodiment 1:
A kind of colloidal sol-gel synthesizing blender is stablized the method for tetragonal phase zirconium oxide nano powder, and it comprises the steps:
(1) configuration ZrOCl
28H
2o and Ce (NO
3)
36H
2the mixing solutions of O, solvent is the mixture of dehydrated alcohol and deionized water, the volume ratio of dehydrated alcohol and deionized water is 1:3, and add a certain amount of Surfactant PEG 600, obtain mixing solutions, wherein the concentration of the amount of substance of zirconium ion is 0.425mol/L, and the concentration of the amount of substance of cerium ion is 0.075mol/L, and the mass percent concentration of PEG600 is 2wt%;
(2) configuration complexing agent citric acid (C
6h
8o
7h
2o) solution, solvent is the mixture of dehydrated alcohol and deionized water, the volume ratio of dehydrated alcohol and deionized water is 1:3,, the amount of substance concentration of citric acid is 0.6mol/L;
(3) step (1) is obtained in solution that solution is dropwise added drop-wise to step (2), the volume ratio that wherein adds step (1) solution and step (2) solution is 1:1, and drop rate is 2ml/min, fully stirs and obtains mixing solutions;
(4) above-mentioned mixing solutions is carried out under agitation condition to heating in water bath, water bath heating temperature is 92
oc, churning time is 72 h;
(5) gel obtaining after heating in water bath being placed in to baking oven is dried; Drying temperature is 120
oc, be 10 h time of drying;
(6) through dried gel after grinding, with 3
othe temperature rise rate of C/min is warming up to 700
oc, afterwards, at this temperature lower calcination 2h, obtains the stably-doped tetragonal phase zirconium oxide nano powder of cerium.
The stably-doped tetragonal phase zirconium oxide nanometer powder that the present embodiment is obtained carries out XRD test, from Fig. 1 result: the thing of synthetic product is Ce mutually
0.84zr
0.16o
2, be the stably-doped tetragonal zircite phase of cerium, there is broadening to a certain extent in diffraction peak simultaneously, shows that synthetic product particle diameter is less.
Stably-doped acquisition tetragonal phase zirconium oxide nanometer powder is carried out to TEM test (Fig. 2), and as shown in Figure 2: synthetic product is near-spherical particle, its particle diameter mean size is 10 ~ 20 nm.
Embodiment 2:
A kind of colloidal sol-gel synthesizing blender is stablized the method for tetragonal phase zirconium oxide nano powder, and it comprises the steps:
(1) configuration ZrOCl
28H
2o and Ce (NO
3)
36H
2the mixing solutions of O, solvent is the mixture of dehydrated alcohol and deionized water, the volume ratio of dehydrated alcohol and deionized water is 1:3, and add a certain amount of Surfactant PEG 600, obtain mixing solutions, wherein the concentration of the amount of substance of zirconium ion is 0.475mol/L, and the concentration of the amount of substance of cerium ion is 0.025mol/L, and the mass percent concentration of PEG600 is 2.8wt%;
(2) configuration complexing agent citric acid (C
6h
8o
7h
2o) solution, solvent is the mixture of dehydrated alcohol and deionized water, the volume ratio of dehydrated alcohol and deionized water is 1:3,, the amount of substance concentration of citric acid is 0.5mol/L;
(3) step (1) is obtained in solution that solution is dropwise added drop-wise to step (2), the volume ratio that wherein adds step (1) solution and step (2) solution is 1:1, and drop rate is 2ml/min, fully stirs and obtains mixing solutions;
(4) above-mentioned mixing solutions is carried out under agitation condition to heating in water bath, water bath heating temperature is 95
oc, churning time is 72 h;
(5) gel obtaining after heating in water bath being placed in to baking oven is dried; Drying temperature is 120
oc, be 10 h time of drying;
(6) through dried gel after grinding, with 3
othe temperature rise rate of C/min is warming up to 750
oc, afterwards, at this temperature lower calcination 2h, obtains the stably-doped tetragonal phase zirconium oxide nano powder of cerium.
The stably-doped tetragonal phase zirconium oxide nanometer powder that the present embodiment is obtained carries out TEM test, can obtain as near-spherical particle synthetic product, and its particle diameter mean size is 10 ~ 20 nm.
Embodiment 3:
A kind of colloidal sol-gel synthesizing blender is stablized the method for tetragonal phase zirconium oxide nano powder, and it comprises the steps:
(1) configuration ZrOCl
28H
2o and Ce (NO
3)
36H
2the mixing solutions of O, solvent is the mixture of dehydrated alcohol and deionized water, the volume ratio of dehydrated alcohol and deionized water is 1:4, and add a certain amount of Surfactant PEG 600, obtain mixing solutions, wherein the concentration of the amount of substance of zirconium ion is 0.45mol/L, and the concentration of the amount of substance of cerium ion is 0.05mol/L, and the mass percent concentration of PEG600 is 4.2wt%;
(2) configuration complexing agent citric acid (C
6h
8o
7h
2o) solution, solvent is the mixture of dehydrated alcohol and deionized water, the volume ratio of dehydrated alcohol and deionized water is 1:4,, the amount of substance concentration of citric acid is 0.6mol/L;
(3) step (1) is obtained in solution that solution is dropwise added drop-wise to step (2), the volume ratio that wherein adds step (1) solution and step (2) solution is 1:1, and drop rate is 2ml/min, fully stirs and obtains mixing solutions;
(4) above-mentioned mixing solutions is carried out under agitation condition to heating in water bath, water bath heating temperature is 90
oc, churning time is 72 h;
(5) gel obtaining after heating in water bath being placed in to baking oven is dried; Drying temperature is 120
oc, be 10 h time of drying;
(6) through dried gel after grinding, with 3
othe temperature rise rate of C/min is warming up to 780
oc, afterwards, at this temperature lower calcination 2h, obtains the stably-doped tetragonal phase zirconium oxide nano powder of cerium.
The stably-doped tetragonal phase zirconium oxide nanometer powder that the present embodiment is obtained carries out XRD test (Fig. 3), from Fig. 3 result: the thing of synthetic product synthetic product is Ce mutually
0.9zr
0.1o
2, be the stably-doped tetragonal zircite phase of cerium, there is broadening to a certain extent in diffraction peak simultaneously, shows that synthetic product particle diameter is less.
The stably-doped tetragonal phase zirconium oxide nanometer powder that the present embodiment is obtained carries out TEM test, can obtain as near-spherical particle synthetic product, and particle mean size is 10 ~ 20 nm.
Embodiment 4:
A kind of colloidal sol-gel synthesizing blender is stablized the method for tetragonal phase zirconium oxide nano powder, and it comprises the steps:
(1) configuration ZrOCl
28H
2o and Ce (NO
3)
36H
2the mixing solutions of O, solvent is the mixture of dehydrated alcohol and deionized water, the volume ratio of dehydrated alcohol and deionized water is 1:3, and add a certain amount of Surfactant PEG 600, obtain mixing solutions, wherein the concentration of the amount of substance of zirconium ion is 0.46mol/L, and the concentration of the amount of substance of cerium ion is 0.04mol/L, and the mass percent concentration of PEG600 is 4wt%;
(2) configuration complexing agent citric acid (C
6h
8o
7h
2o) solution, solvent is the mixture of dehydrated alcohol and deionized water, the volume ratio of dehydrated alcohol and deionized water is 1:3,, the amount of substance concentration of citric acid is 0.6mol/L;
(3) step (1) is obtained in solution that solution is dropwise added drop-wise to step (2), the volume ratio that wherein adds step (1) solution and step (2) solution is 1:1, and drop rate is 2ml/min, fully stirs and obtains mixing solutions;
(4) above-mentioned mixing solutions is carried out under agitation condition to heating in water bath, water bath heating temperature is 94
oc, churning time is 72 h;
(5) gel obtaining after heating in water bath being placed in to baking oven is dried; Drying temperature is 120
oc, be 10 h time of drying;
(6) through dried gel after grinding, with 3
othe temperature rise rate of C/min is warming up to 750
oc, afterwards, at this temperature lower calcination 2h, obtains the stably-doped tetragonal phase zirconium oxide nano powder of cerium.
The stably-doped tetragonal phase zirconium oxide nanometer powder that the present embodiment is obtained carries out TEM test, can obtain as near-spherical particle synthetic product, and particle mean size is 10 ~ 20 nm.
Embodiment 5:
Sol-gel processing synthesizing blender is stablized a method for tetragonal phase zirconium oxide nano powder, and it comprises the steps:
(1) configuration ZrOCl
28H
2o and Ce (NO
3)
36H
2the mixing solutions of O, solvent is the mixture of dehydrated alcohol and deionized water, the volume ratio of dehydrated alcohol and deionized water is 1:4, and add a certain amount of Surfactant PEG 600, obtain mixing solutions, wherein the concentration of the amount of substance of zirconium ion is 0.44mol/L, and the concentration of the amount of substance of cerium ion is 0.06mol/L, and the mass percent concentration of PEG600 is 5wt%;
(2) configuration complexing agent citric acid (C
6h
8o
7h
2o) solution, solvent is the mixture of dehydrated alcohol and deionized water, the volume ratio of dehydrated alcohol and deionized water is 1:4,, the amount of substance concentration of citric acid is 0.6mol/L;
(3) step (1) is obtained in solution that solution is dropwise added drop-wise to step (2), the volume ratio that wherein adds step (1) solution and step (2) solution is 1:1, and drop rate is 2ml/min, fully stirs and obtains mixing solutions;
(4) above-mentioned mixing solutions is carried out under agitation condition to heating in water bath, water bath heating temperature is 94
oc, churning time is 72 h;
(5) gel obtaining after heating in water bath being placed in to baking oven is dried; Drying temperature is 120
oc, be 12h time of drying;
(6) through dried gel after grinding, with 3
othe temperature rise rate of C/min is warming up to 800
oc, afterwards, at this temperature lower calcination 2h, obtains the stably-doped tetragonal phase zirconium oxide nano powder of cerium.
The stably-doped tetragonal phase zirconium oxide nanometer powder that the present embodiment is obtained carries out TEM test, can obtain as near-spherical particle synthetic product, and its particle diameter mean size is 10 ~ 20 nm.
Claims (6)
1. the method for the synthetic stably-doped tetragonal phase zirconium oxide nano powder of cerium of sol-gel method, is characterized in that, synthesis step is:
(1) under room temperature, getting He Shi source, soluble zirconium source is dissolved in solvent, afterwards, add again tensio-active agent, after being fully uniformly mixed, making containing zirconium ion concentration is 0.425-0.475 mol/L, and cerium ion concentration is 0.025-0.075 mol/L, tensio-active agent mass concentration is 2 ~ 5% mixed solution A, for subsequent use;
(2) separately get a certain amount of solvent, add wherein complexing agent, after fully stirring, dissolving, making containing complexing agent concentration is the mixing solutions B of 0.5-0.6 mol/L, for subsequent use;
(3) by volume umber is got respectively the mixing solutions B that mixed solution A that 1 part of step (1) makes and 1 part of step (2) make, under agitation condition, the mixed solution A obtaining is added dropwise in mixing solutions B with the speed of 2ml/min, and the mixing solutions obtaining after fully mixing is for subsequent use;
(4), under agitation condition, it is 90 ~ 95 that the mixing solutions that step (3) is obtained is put into temperature
oin the water-bath of C, carry out heating in water bath 72 h, obtain gel;
(5) gel step (4) being obtained is put into 120-130
oin the loft drier of C, be dried 10-12 h, obtain solid xerogel;
(6), after solid xerogel step (5) being obtained grinds, transposition enters in muffle furnace, is warming up to 700 ~ 800
oc, 700 ~ 800
ounder C condition, calcine 2h, obtain the stable tetragonal phase zirconium oxide nano powder of cerium doping.
2. the method for the synthetic stably-doped tetragonal phase zirconium oxide nano powder of cerium of sol-gel method according to claim 1, is characterized in that: the zirconium source described in step 1) is ZrOCl
28H
2o, cerium source is Ce (NO
3)
36H
2o, tensio-active agent is PEG600.
3. the method for the synthetic stably-doped tetragonal phase zirconium oxide nano powder of cerium of sol-gel method according to claim 1, it is characterized in that: in step (1) and step (2), described solvent is that volume ratio is the deionized water of 3 ~ 4:1 and the mixed solution of dehydrated alcohol.
4. the method for the synthetic stably-doped tetragonal phase zirconium oxide nano powder of cerium of the sol-gel method stated according to claim 1, is characterized in that: step 2) described complexing agent is C
6h
8o
7h
2o.
5. the method for the synthetic stably-doped tetragonal phase zirconium oxide nano powder of cerium of sol-gel method according to claim 1, is characterized in that: the drying temperature described in step 5) is 120
oc, be 10 h time of drying.
6. the method for the synthetic stably-doped tetragonal phase zirconium oxide nano powder of cerium of sol-gel method according to claim 1, is characterized in that: in step 6) with 3
othe temperature rise rate of C/min is warming up to 700 ~ 800
oc.
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