CN101825551B - Cerium dioxide microsphere used as dimension standard material - Google Patents
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Abstract
The invention relates to the technical field of the quantity transmission of the measuring and testing standard. Particularly, the invention relates to a cerium dioxide microsphere used as a dimension standard material. The cerium dioxide microsphere is an inorganic-organic hybrid microsphere and consists of cerium dioxide and polyvinylpyrrolidone molecules, wherein the weight ratio of cerium dioxide to polyvinylpyrrolidone is 11-16:1; the inorganic-organic hybrid microsphere is of a polycrystalline structure and belongs to the cubic system; the crystal structure is fluorspar structure; the structure cell is of a face-centred cubic structure; the shape factor of the microsphere is less than 1.2; and the relative uncertaitny of the dimension value is less than 5 percent. The cerium dioxide microsphere in the submicron/nano level, which is provided by the invention and is used as the granularity standard material, has the advantages of large proportion, high temperature resistance and acid and alkali resistance, does not swell in the organic solvent, is not easy to be eroded by germs and has the specific crystal structure.
Description
Technical field
The present invention relates to the technical field of metrology and measurement standard transmission of quantity value, more particularly, the present invention relates to a kind of cerium dioxide micro-balloon as dimension standard material.
Background technology
Development along with powder technology and nanosecond science and technology, the submicron powder has attracted increasing sight, its development and application potential are unquestionable, therefore urgent day by day to the detection demand of submicron yardstick powder, various granulometry technology that adapt therewith and instrument are also constantly progressive.But because the complicacy that granularity characterizes, no matter which kind of principle granulometry follows, and the granulometry means need submicron level granulometry material (SRM) to proofread and correct or verify bar none.In addition, in the research of colloidal dispersion, submicron level granulometry material is still measured the instrument that makes things convenient for of bacterium, virus, ribosomes and cellule material size.The granulometry material belongs to engineering feature measurement standard substance.
The submicron level granulometry material that uses in the world comprises monodispersed polystyrene microsphere at present, and as 1960,1961,1963 and No. 1964 polystyrene microspheres, the concentration that is dispersed in the water is about 0.5wt%, and SiO
2Microballoon, the selectable size scope is at 0.5～1.6 μ m, and the concentration that is dispersed in the water is about 2wt%.
As the granulometry material, polystyrene and silicon dioxide microsphere have lot of advantages, still, and the low (1.06g/cm of organism polystyrene density
3), too small with the density difference of water, easy swelling in organic solvent, non-refractory, polystyrene is subject to the bacterium erosion in addition; And silicon dioxide belongs to amorphous state, not alkaline-resisting and hydrofluorite, and hydrothermal stability is relatively poor.
Hydro-thermal method is in special closed reaction vessel autoclave, adopt aqueous solution as reaction medium, by to reaction vessel heating, create the reaction environment of a High Temperature High Pressure, make common indissoluble or insoluble substance dissolves and recrystallization and make the crystalline particle product.Hydro-thermal method and other ceria preparation method main difference point have: hydro-thermal method is directly prepared crystalline particle from solution; Can be by the pattern and the crystalline phase of initial substance precursor control powder granule; Usually the granular product that need not calcination and process of lapping and obtain hanging down degree of aggregation.It is a lot of that cerium salt sediment is carried out the research report that hydrothermal crystallizing prepares cerium oxide particles, but simple hydrothermal method obtains the nano ceric oxide grain graininess and the pattern controllable degree is low.
The technology that common template prepares ceria is to add the template agent in the precipitation reaction of cerium salt, obtain cerium dioxide nano line, nanometer rods or nano particle by calcining then, then sediment is calcined as cerous acetate is refluxed in propylene glycol, made the cerium dioxide micro-balloon about particle diameter 1 μ m.This class is based on the technology of precipitation calcining, and the particle reunion degree height that obtains, pattern be rule inadequately.
Also has report, under hydrothermal condition, induce cerous nitrate hydrolysis nucleation crystallization to make submicron order polycrystalline cerium dioxide micro-balloon with the different templates agent, this process combines template with hydro-thermal, made the higher cerium oxide particle of sphericity, but the homogeneity of particle size is still relatively poor.
Therefore, the synthetic research of ceria spheric grain control at present is also very immature, obtain sphericity and the good cerium oxide particles of monodispersity also needs to explore new synthesis technique in sub-micron, nanoscale scope.The present invention proposes a kind of composite shuttering crystal seed induces hydro-thermal method to come single cerium dioxide micro-balloon that disperses of controlledly synthesis size homogeneous.
Summary of the invention
The purpose of this invention is to provide a kind of cerium dioxide micro-balloon as dimension standard material.
Cerium dioxide micro-balloon provided by the invention is the inorganic-organic hybridization microballoon, form by ceria and polyvinylpyrrolidonemolecules molecules, wherein the weight ratio of ceria and polyvinylpyrrolidone is 11～16: 1, this inorganic-organic hybridization microballoon is a polycrystalline structure, belongs to cubic system, and crystal structure is fluorite type (as shown in Figure 1), structure cell is a face-centred cubic structure, the microballoon form factor is less than 1.2, and range of size is 90nm～450nm, and the relative uncertainty of size value is less than 5%.
The present invention is on template and basis that hydro-thermal method combines, having proposed a kind of composite shuttering crystal seed induces hydro-thermal method to come the single cerium dioxide micro-balloon that disperses of controlledly synthesis, by prepared inorganic-organic composite shuttering is as crystal seed, evenly induce cerium salt hydrolysis nucleation, strengthen hydrothermal crystallization process, by to synthetic parameter control, obtain the monodisperse spherical cerium oxide particles of serial size homogeneous.
Therefore, the invention provides a kind of cerium dioxide micro-balloon, its method preparation by may further comprise the steps:
1) hydro-thermal reaction for the first time: mix cerium salt, polyvinylpyrrolidone and water, after the stirring and dissolving, move in the water heating kettle, at 140～280 ℃ of following stirring reaction 12～48h, the centrifugal acquisition supernatant in cooling back, wherein, cerium salt is 1: 0.5～3 with the initial mass ratio of polyvinylpyrrolidone, and cerium salt initial concentration is 0.09～0.18mol/L; And
2) hydro-thermal reaction for the second time: in the supernatant that obtains, add cerium salt, after stirring, move in the water heating kettle, at 140～280 ℃ of following stirring reaction 12～48h, through cooling, centrifugal, cleaning acquisition cerium dioxide micro-balloon, wherein, the concentration of described cerium salt is 0.03～0.06mol/L then.
According to cerium dioxide micro-balloon of the present invention, described cerium salt is for easily being dissolved in the cerous salt of water, the molecular weight of described polyvinylpyrrolidone is 8000～360000, comprises PVP K15, PVP K17, PVP K25, PVP K30, PVP K40, PVP K60 and PVP K90; The water heating kettle compactedness is 50～80%; The rotating speed that stirs in twice hydro-thermal reaction is 10～800rpm.
Particularly, at first, cerium salt, polyvinylpyrrolidone and water mixed by a certain percentage carry out the hydro-thermal reaction first time.Behind the reaction natural cooling, this reaction product mixed liquor is carried out liquid-solid separation, earlier at high speed centrifugation reaction product mixed liquor, particle is sunken to the centrifuge tube bottom, supernatant liquor is slowly poured in the centrifuge tube that prior cleaning handled, to supernatant liquor once more at high speed centrifugation, this process repeats more than twice or twice at least, resulting upper strata liquid is inorganic-organic composite shuttering liquid, wherein cerium oxide crystal seed and pyrrolidone ring interact, be embedded in the polyvinylpyrrolidonemolecules molecules chain, form inorganic organic composite shuttering, be uniformly distributed in the whole reaction system.
Then, to slowly pour in the clean container of preprepared through the supernatant of centrifugal treating, to wherein adding a certain amount of cerium salt, evenly behind the mixed dissolution, carry out the secondary hydro-thermal reaction, initiate cerium molecules of salt under the inducing of crystal seed, homogeneous nucleation in whole system, crystal growth under condition much at one.Behind the natural cooling, this reaction product mixed liquor is carried out liquid-solid separation, elder generation's high speed centrifugation reaction product mixed liquor, particle is sunken to the centrifuge tube bottom, removes upper strata liquid, injects deionized water in centrifuge tube, centrifugal once more after mixing, so repeatedly the resulting granules thing is carried out centrifuge washing more than three times or three times, finally press the desired concn ratio, particle is dispersed in aqueous phase.
In the above-mentioned steps, when the hydro-thermal reaction product was carried out liquid-solid separation and particle centrifuge washing, the rotating speed of supercentrifuge was at least 10000rpm, and centrifuging temperature is at-4～0 ℃, and the single centrifugation time is at least 20min.
The particle dispersion that obtains is bottled, grab sample in some bottles of samples, adopt high-precision laser particle analyzer, according to " ISO Guide 35:2006, Reference materials-General andstatistical principles for certification, IDT " and the principle of " rule and the statistical method of GB/T 15000.3-2008 standard model work guide rule (3) standard model definite value " sample unit is carried out the monitoring and evaluation and the definite value of homogeneity and stability, according to National Standard ISO 13322-1 Particle sizeanalysis-Image analysis methods-Part 1:Static image analysis methods " and the method principle of " GB/T 21649.1-2008 sreen analysis image analytical method part 1: still image analytic approach ", take the method for transmission electron microscope Duo Jia laboratory associating definite value that particle size is carried out definite value, and carry out uncertain analysis according to " JCGM 100:2008 Evaluation of measurement data-Guide to the expressionof uncertainty in measurement " and the principle of " JJF1059-1999 evaluation of uncertainty in measurement and expression ".
Other cerium dioxide micro-balloon of submicron level that the invention provides is as the granulometry material, its than in great, high temperature resistant, acid and alkali-resistance, the organic solvent not swelling, be not subject to bacterium and corrode, have specific crystal structure.Also do not have in the world at present the inorganic oxide microsphere particle of tool crystal structure report as submicron rank dimension standard material.Cerium dioxide micro-balloon sphericity of the present invention and monodispersity good (seeing Fig. 2 and Fig. 3), the relative uncertainty of size value is less than 5%, and form factor is less than 1.2.
Description of drawings
Fig. 1 is prepared cerium oxide microsphere particle XRD diffracting spectrum;
Fig. 2 is prepared cerium oxide microsphere particle TEM photo;
Fig. 3 is prepared cerium oxide microsphere particle SEM photo.
Embodiment
Embodiment 1
19.6g cerous nitrate, 9.8g polyvinylpyrrolidone (K90) and 400g water are mixed, after the stirring and dissolving, be diluted to 500mL, pour in the water heating kettle of 1000mL, setting hydrothermal temperature is 140 ℃, rotating speed 800rpm, carries out the hydro-thermal reaction first time, stops reaction behind the 48h.After the cooling of question response still, with this reaction product mixed liquor centrifugal 20min under the centrifugal rotational speed of-4 ℃ centrifuging temperature and 10000rpm, particle is sunken to the centrifuge tube bottom, supernatant liquor slowly poured in the centrifuge tube that prior cleaning handled collect and discarded bottom particle, to supernatant liquor high speed centrifugation 20min under same temperature and rotating speed once more, remove centrifuge tube bottom particle, collect supernatant liquor, so repeated treatments twice gets supernatant liquor and is inorganic organic composite shuttering liquid.Composite shuttering liquid is poured in the clean container of preprepared, be settled to 500mL, to wherein adding the 6.5g cerous nitrate with deionized water, after the stirring and dissolving, pour in the water heating kettle of 1000mL, setting hydrothermal temperature is 140 ℃, rotating speed 800rpm, carry out the secondary hydro-thermal reaction, stop reaction behind the 48h.After the cooling of question response still, with this reaction product mixed liquor centrifugal 20min under the centrifugal rotational speed of-4 ℃ centrifuging temperature and 10000rpm, collection is sunken to the particle of centrifuge tube bottom, remove upper strata liquid, in centrifuge tube, inject deionized water, mix back centrifugal once more 20min under same condition, so repeatedly the resulting granules thing is carried out centrifuge washing three times, finally be made into the aqueous dispersions that concentration is 0.5wt%, bottling.
According to " ISO Guide 35:2006; Reference materials-General and statisticalprinciples for certification; IDT " and the principle of " rule and the statistical method of GB/T 15000.3-2008 standard model work guide rule (3) standard model definite value ", adopt high-precision laser particle analyzer sample unit to be carried out the monitoring and evaluation of homogeneity and stability, grab sample in some bottles of samples, carrying out homogeneity detects, take a sample test 15 bottles of samples at random, each sample measurement three times, 45 data of gained are carried out the characteristic value statistical study, the Rod Dixon criterion judges that above-mentioned data do not have outlier, through F check no significant difference, have good uniformity.The principle of taking earlier close back to dredge is got 6 time points in the time of a year and a half, the sample of randomly drawing is carried out stability test, and resulting performance data is through t testing identity no significant difference, and explanation had good stability, above 1 year. is according to the Method And Principle of GB " ISO 13322-1 Particle size analysis-Image analysis methods-Part 1:Static image analysis methods " and " GB/T 21649.1-2008 grain size analysis image analytical method part 1: still image analytic approach "; Take the method for transmission electron microscope Duo Jia laboratory associating definite value that particle size is carried out definite value, and carry out uncertain analysis according to " JCGM 100:2008 Evaluation ofmeasurement data-Guide to the expression of uncertainty in measurement " and the principle of " JJF1059-1999 evaluation of uncertainty in measurement and expression ". Resulting cerium oxide dimensional standard microballoon value and uncertainty thereof are:(90.6 ± 3.1) nm, uncertainty is 3.4% relatively.The microballoon form factor is 1.07.Utilize thermal gravimetric analyzer that microsphere particle is analyzed, wherein the weight ratio of ceria and polyvinylpyrrolidone is 16:1.
Embodiment 2
55.6g cerous nitrate, 48.5g polyvinylpyrrolidone (K30) and 650g water are mixed, after the stirring and dissolving, be diluted to 800mL, pour in the water heating kettle of 1000mL, setting hydrothermal temperature is 170 ℃, rotating speed 25rpm, carries out the hydro-thermal reaction first time, stops reaction behind the 24h.After the cooling of question response still, with this reaction product mixed liquor centrifugal 20min under the centrifugal rotational speed of-3 ℃ centrifuging temperature and 10000rpm, particle is sunken to the centrifuge tube bottom, supernatant liquor slowly poured in the centrifuge tube that prior cleaning handled collect and discarded bottom particle, to supernatant liquor high speed centrifugation 20min under same temperature and rotating speed once more, remove centrifuge tube bottom particle, collect supernatant liquor, so repeated treatments twice gets supernatant liquor and is inorganic organic composite shuttering liquid.Composite shuttering liquid is poured in the clean container of preprepared, be settled to 800mL, to wherein adding the 13.8g cerous nitrate with deionized water, after the stirring and dissolving, pour in the water heating kettle of 1000mL, setting hydrothermal temperature is 160 ℃, rotating speed 15rpm, carry out the secondary hydro-thermal reaction, stop reaction behind the 24h.After the cooling of question response still, with this reaction product mixed liquor centrifugal 20min under the centrifugal rotational speed of-3 ℃ centrifuging temperature and 10000rpm, collection is sunken to the particle of centrifuge tube bottom, remove upper strata liquid, in centrifuge tube, inject deionized water, mix back centrifugal once more 20min under same condition, so repeatedly the resulting granules thing is carried out centrifuge washing three times, finally be made into the aqueous dispersions that concentration is 0.5wt%, bottling.
Carry out the homogeneity detection according to the method principle that embodiment 1 mentions, take a sample test 15 bottles of samples at random, each sample measurement three times, 45 data of gained are carried out the characteristic value statistical study, the Rod Dixon criterion judges that above-mentioned data do not have outlier, through F check no significant difference, has good uniformity.The principle of taking earlier close back to dredge is got 6 time points in the time of a year and a half, the sample of randomly drawing is carried out stability test, and resulting performance data is through t testing identity no significant difference, and explanation had good stability, above 1 year.Carry out definite value and analysis on Uncertainty according to the method principle that embodiment 1 mentions, embodiment 2 resulting cerium oxide dimensional standard microballoon values and uncertainty thereof are: (152.7 ± 4.3) nm, uncertainty is 2.8% relatively.The microballoon form factor is 1.14.Utilize thermal gravimetric analyzer that microsphere particle is analyzed, wherein the weight ratio of ceria and polyvinylpyrrolidone is 15: 1.
Embodiment 3
158.8g cerium chloride, 165.3g polyvinylpyrrolidone (K60) and 1900g water are mixed, after the stirring and dissolving, be diluted to 2100mL, pour in the water heating kettle of 3000mL, setting hydrothermal temperature is 180 ℃, rotating speed 450rpm, carries out the hydro-thermal reaction first time, stops reaction behind the 36h.After the cooling of question response still, with this reaction product mixed liquor centrifugal 25min under the centrifugal rotational speed of 0 ℃ centrifuging temperature and 20000rpm, particle is sunken to the centrifuge tube bottom, supernatant liquor slowly poured in the centrifuge tube that prior cleaning handled collect and discarded bottom particle, to supernatant liquor high speed centrifugation 25min under same temperature and rotating speed once more, remove centrifuge tube bottom particle, collect supernatant liquor, so repeated treatments twice gets supernatant liquor and is inorganic organic composite shuttering liquid.Composite shuttering liquid is poured in the clean container of preprepared, to wherein adding the 30g cerium chloride, after the stirring and dissolving, be settled to 2100mL with deionized water, pour in the water heating kettle of 2000mL, setting hydrothermal temperature is 170 ℃, rotating speed 400rpm, carry out the secondary hydro-thermal reaction, stop reaction behind the 30h.After the cooling of question response still, with this reaction product mixed liquor centrifugal 25min under the centrifugal rotational speed of 0 ℃ centrifuging temperature and 20000rpm, collection is sunken to the particle of centrifuge tube bottom, remove upper strata liquid, in centrifuge tube, inject deionized water, mix back centrifugal once more 25min under same condition, so repeatedly the resulting granules thing is carried out centrifuge washing three times, finally be made into the aqueous dispersions that concentration is 0.4wt%, bottling.
Carry out the homogeneity detection according to the method principle that embodiment 1 mentions, take a sample test 15 bottles of samples at random, each sample measurement three times, 45 data of gained are carried out the characteristic value statistical study, the Rod Dixon criterion judges that above-mentioned data do not have outlier, through F check no significant difference, has good uniformity.The principle of taking earlier close back to dredge is got 6 time points in the time of a year and a half, the sample of randomly drawing is carried out stability test, and resulting performance data is through t testing identity no significant difference, and explanation had good stability, above 1 year.Carry out definite value and analysis on Uncertainty according to the method principle that embodiment 1 mentions, embodiment 3 resulting cerium oxide dimensional standard microballoon values and uncertainty thereof are: (350.7 ± 6.1) nm, uncertainty is 1.7% relatively.The microballoon form factor is 1.15.Utilize thermal gravimetric analyzer that microsphere particle is analyzed, wherein the weight ratio of ceria and polyvinylpyrrolidone is 13: 1.
Embodiment 4
125g cerous nitrate, 375g polyvinylpyrrolidone (K15) and 1200g water are mixed, after the stirring and dissolving, be diluted to 1600mL, pour in the water heating kettle of 2000mL, setting hydrothermal temperature is 280 ℃, rotating speed 10rpm, carries out the hydro-thermal reaction first time, stops reaction behind the 12h.After the cooling of question response still, with this reaction product mixed liquor centrifugal 25min under the centrifugal rotational speed of 0 ℃ centrifuging temperature and 20000rpm, particle is sunken to the centrifuge tube bottom, supernatant liquor slowly poured in the centrifuge tube that prior cleaning handled collect and discarded bottom particle, to supernatant liquor high speed centrifugation 25min under same temperature and rotating speed once more, remove centrifuge tube bottom particle, collect supernatant liquor, so repeated treatments twice gets supernatant liquor and is inorganic organic composite shuttering liquid.Composite shuttering liquid is poured in the clean container of preprepared, be settled to 1600mL, to wherein adding the 41.6g cerous nitrate with deionized water, after the stirring and dissolving, pour in the water heating kettle of 2000mL, setting hydrothermal temperature is 280 ℃, rotating speed 10rpm, carry out the secondary hydro-thermal reaction, stop reaction behind the 12h.After the cooling of question response still, with this reaction product mixed liquor centrifugal 25min under the centrifugal rotational speed of 0 ℃ centrifuging temperature and 20000rpm, collection is sunken to the particle of centrifuge tube bottom, remove upper strata liquid, in centrifuge tube, inject deionized water, mix back centrifugal once more 25min under same condition, so repeatedly the resulting granules thing is carried out centrifuge washing three times, finally be made into the aqueous dispersions that concentration is 0.3wt%, bottling.
Carry out the homogeneity detection according to the method principle that embodiment 1 mentions, take a sample test 15 bottles of samples at random, each sample measurement three times, 45 data of gained are carried out the characteristic value statistical study, the Rod Dixon criterion judges that above-mentioned data do not have outlier, through F check no significant difference, has good uniformity.The principle of taking earlier close back to dredge is got 6 time points in the time of a year and a half, the sample of randomly drawing is carried out stability test, and resulting performance data is through t testing identity no significant difference, and explanation had good stability, above 1 year.Carry out definite value and analysis on Uncertainty according to the method principle that embodiment 1 mentions, embodiment 2 resulting cerium oxide dimensional standard microballoon values and uncertainty thereof are: (450.8 ± 7.1) nm, uncertainty is 1.6% relatively.The microballoon form factor is 1.16.Utilize thermal gravimetric analyzer that microsphere particle is analyzed, wherein the weight ratio of ceria and polyvinylpyrrolidone is 11: 1.
Claims (8)
1. cerium dioxide micro-balloon as dimension standard material, it is characterized in that, described cerium dioxide micro-balloon is the inorganic-organic hybridization microballoon, form by ceria and polyvinylpyrrolidonemolecules molecules, wherein the weight ratio of ceria and polyvinylpyrrolidone is 11～16: 1, this inorganic-organic hybridization microballoon is a polycrystalline structure, belong to cubic system, crystal structure is a fluorite type, structure cell is a face-centred cubic structure, the microballoon form factor is less than 1.2, and range of size is 90nm～450nm, and the relative uncertainty of size value is less than 5%.
2. the cerium dioxide micro-balloon as dimension standard material according to claim 1 is characterized in that, the method preparation of described cerium dioxide micro-balloon by may further comprise the steps:
1) hydro-thermal reaction for the first time: mix cerium salt, polyvinylpyrrolidone and water, after the stirring and dissolving, move in the water heating kettle, at 140～280 ℃ of following stirring reaction 12～48h, the centrifugal acquisition supernatant in cooling back, wherein, cerium salt is 1: 0.5～3 with the initial mass ratio of polyvinylpyrrolidone, and cerium salt initial concentration is 0.09～0.18mol/L; And
2) hydro-thermal reaction for the second time: in the supernatant that obtains, add cerium salt, after stirring, move in the water heating kettle, at 140～280 ℃ of following stirring reaction 12～48h, through cooling, centrifugal, cleaning acquisition cerium dioxide micro-balloon, wherein, the concentration of described cerium salt is 0.03～0.06mol/L then.
3. cerium dioxide micro-balloon according to claim 2 is characterized in that, described cerium salt is for easily being dissolved in the cerous salt of water.
4. cerium dioxide micro-balloon according to claim 3 is characterized in that, described cerium salt is cerous nitrate or cerium chloride.
5. cerium dioxide micro-balloon according to claim 2 is characterized in that, the molecular weight of described polyvinylpyrrolidone is 8000～360000.
6. cerium dioxide micro-balloon according to claim 5 is characterized in that, described polyvinylpyrrolidone is PVP K15, PVP K17, PVP K25, PVP K30, PVP K40, PVP K60 or PVP K90.
7. cerium dioxide micro-balloon according to claim 2 is characterized in that, the water heating kettle compactedness is 50～80%.
8. cerium dioxide micro-balloon according to claim 2 is characterized in that, the rotating speed that stirs in twice hydro-thermal reaction is 10～800rpm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005247673A (en) * | 2004-03-08 | 2005-09-15 | National Institute For Materials Science | Dy-DOPED NANO CERIA SINTERED COMPACT AND ITS MANUFACTURING METHOD |
| CN101117233A (en) * | 2007-07-23 | 2008-02-06 | 北京科技大学 | Method for preparing high specific surface area meso-porous cerium dioxide micro-balloon |
| CN101244837A (en) * | 2008-03-13 | 2008-08-20 | 同济大学 | Method for manufacturing high purity nano-cerium dioxide |
| CN101825552A (en) * | 2009-07-23 | 2010-09-08 | 中国科学院过程工程研究所 | Method for preparing cerium dioxide microsphere used as dimension standard material |
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| JP2005247673A (en) * | 2004-03-08 | 2005-09-15 | National Institute For Materials Science | Dy-DOPED NANO CERIA SINTERED COMPACT AND ITS MANUFACTURING METHOD |
| CN101117233A (en) * | 2007-07-23 | 2008-02-06 | 北京科技大学 | Method for preparing high specific surface area meso-porous cerium dioxide micro-balloon |
| CN101244837A (en) * | 2008-03-13 | 2008-08-20 | 同济大学 | Method for manufacturing high purity nano-cerium dioxide |
| CN101825552A (en) * | 2009-07-23 | 2010-09-08 | 中国科学院过程工程研究所 | Method for preparing cerium dioxide microsphere used as dimension standard material |
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