CN106477586A - For calibrating nano particle size standard substance of granulometry and preparation method thereof - Google Patents
For calibrating nano particle size standard substance of granulometry and preparation method thereof Download PDFInfo
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- CN106477586A CN106477586A CN201610900591.7A CN201610900591A CN106477586A CN 106477586 A CN106477586 A CN 106477586A CN 201610900591 A CN201610900591 A CN 201610900591A CN 106477586 A CN106477586 A CN 106477586A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 239000000126 substance Substances 0.000 title claims abstract description 28
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 27
- 238000001033 granulometry Methods 0.000 title claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 115
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 25
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 15
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 38
- 238000004140 cleaning Methods 0.000 claims description 25
- 239000008187 granular material Substances 0.000 claims description 23
- 230000003321 amplification Effects 0.000 claims description 22
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 22
- 239000004793 Polystyrene Substances 0.000 claims description 21
- 229920002223 polystyrene Polymers 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000000839 emulsion Substances 0.000 claims description 17
- 239000000377 silicon dioxide Substances 0.000 claims description 13
- 235000012239 silicon dioxide Nutrition 0.000 claims description 13
- 238000005119 centrifugation Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 9
- 238000004513 sizing Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 238000007689 inspection Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 3
- 239000012925 reference material Substances 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000003921 particle size analysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- -1 and that is Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
- G01N15/1012—Calibrating particle analysers; References therefor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
- G01N15/1012—Calibrating particle analysers; References therefor
- G01N2015/1014—Constitution of reference particles
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
- G01N2015/1029—Particle size
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Abstract
The present invention relates to for the nano particle size standard substance calibrating granulometry, being made up of the spheroidal particle that nominal particle size is 80 600nm, described spheroidal particle is spherical.Described nano particle size standard substance is made by following steps：Tetraethyl orthosilicate and ethanol are added in reactor, mixes, and distilled water and ammonia are stirred formation mixed liquor；Described mixed liquor is slowly instilled in described reactor, continuously stirred, completion of dropping, continues the stirring scheduled time, obtains spherical.The nano particle size standard substance of present invention preparation has good sphericity, monodispersity and stability, and disclosure satisfy that the calibration requirements of particle sizing.
Description
Technical field
The invention belongs to standard matter preparing technology field, relate to calibrate the nano particle size standard substance of granulometry
And preparation method thereof, and it is related to a kind of preparation method of the nano particle size standard substance for calibrating granulometry.
Background technology
Powder body material is a kind of new material developed in recent years, and it is in the side such as catalysis, light absorbs, medical treatment, sterilization
Face has the incomparable good characteristic of conventional powder material, is therefore gradually paid attention to by whole world various countries, at present, many
National government all carries out research and the industrialization production of powder body material in the substantial amounts of human and material resources of input and financial resources.But people
The feature of the physicochemical characteristicss of powder body material of concern is exactly the size depending strongly on granule, and that is, powder body material shows
Significantly dimensional effect.The size that this allows for how accurately measuring powder body material becomes preparation, research, application powder body material
Unusual distinct issues.
The whether accurate correction needing reference materials for particle size analysis of testing graininess and calibrating.Particle size standard substance is considered
It is the effective carrier of magnitude tracing and ensure accurate, reliable, the consistent generally acknowledged effective means of granulometry value in granulometry.
At present, abroad many metrological services pay much attention to and have carried out one after another the correlational study of granularity measurement criteria and magnitude tracing system
Work.In order to improve tracing to the source and transport system of granulometry, ensure that China is consistent in the international equivalent of granulometry, the present invention
Disclose a kind of tracing to the source to the nano particle size standard substance of China's measurement criteria, as the supplement of existing reference materials for particle size analysis.
Content of the invention
It is an object of the invention to provide for calibrating nano particle size standard substance of granulometry and preparation method thereof.
The present invention also aims to providing a kind of preparation side of the nano particle size standard substance for calibrating granulometry
Method.
For reaching foregoing invention purpose, on the one hand, the invention provides for the nano particle size standard calibrating granulometry
Material, is made up of the spheroidal particle for 80-600nm for the nominal particle size, and spheroidal particle is spherical.
In addition, above-mentioned nano particle size standard substance makes as follows：Preparation process：By tetraethyl orthosilicate and ethanol
Add in reactor, mix, and distilled water and ammonia are stirred formation mixed liquor；Reactions steps：Mixed liquor is slowly dripped
Enter in reactor, continuously stirred, completion of dropping, continues to stir the scheduled time at a predetermined temperature, obtains spherical of silicon dioxide
Grain emulsion；And cleaning step：Deionized water eccentric cleaning spherical emulsion, obtains spherical of silicon dioxide
Grain.
In addition, the tetraethyl orthosilicate in preparation process can be 5-10mL, ethanol can be 100-150mL, and distilled water can
Think 5-30mL, ammonia can be 10-15mL.
In addition, the stir speed (S.S.) in reactions steps can be 200-400r/min, drop rate can be 0.1-0.5mL/
s.
In addition, the predetermined temperature in reactions steps can be 25-35 DEG C, the scheduled time can be 3h.
In addition, the centrifugation in cleaning step can carry out 8-15min under centrifugation rate is for 6000-9000r/min.
In addition, above-mentioned nano particle size standard substance further by microscopic method come definite value, wherein, by microscopic method Lai
Definite value comprises the steps：Using scanning electron microscope, certain amount of spherical crosslinked polystyrene standard particle is put
Greatly, and one by one shoot the image of spherical crosslinked polystyrene standard particle；Standard micrometer is determined under same amplification
Scale is to determine the area of single pixel under amplification；By calculating the quantity of the pixel that standard particle comprises, determine standard
The equivalent projected area of granule, thus obtain the equivalent diameter projected of standard particle；Measure the particle diameter of each standard particle one by one,
To carry out definite value.
On the other hand, the present invention provides a kind of preparation method of the nano particle size standard substance for calibrating granulometry,
Comprise the following steps：Preparation process：Tetraethyl orthosilicate and ethanol are added in reactor, mixes, and distilled water and ammonia are stirred
Mix and be formed uniformly mixed liquor；Reactions steps：Mixed liquor is slowly instilled in reactor, continuously stirred, completion of dropping, continue pre-
Determine to stir the scheduled time at temperature, obtain spherical emulsion；And cleaning step：Deionized water eccentric cleaning two
The spherical grain emulsion of silicon oxide, obtains spherical.
In addition, above-mentioned preparation method also includes the step by microscopic method come definite value, wherein, determined by microscopic method
Value comprises the steps：Using scanning electron microscope, certain amount of spherical crosslinked polystyrene standard particle is put
Greatly, and one by one shoot the image of spherical crosslinked polystyrene standard particle；Standard micrometer is determined under same amplification
Scale is to determine the area of single pixel under amplification；By calculating the quantity of the pixel that standard particle comprises, determine standard
The equivalent projected area of granule, thus obtain the equivalent diameter projected of standard particle；Measure the particle diameter of each standard particle one by one,
To carry out definite value.
Brief description
Fig. 1 is the preparation process flow chart of silica dioxide granule.
Fig. 2 is the electron scanning micrograph of the spherical of particle diameter 80nm in embodiment 1.
Fig. 3 is the electron scanning micrograph of the spherical of particle diameter 300nm in embodiment 4.
Fig. 4 is the transmission electron microscope photo of the spherical of particle diameter 600nm in embodiment 5.
Specific embodiment
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings, described specific embodiment is only right
The present invention explains, and is not limited to the present invention.
According to the embodiment of the present invention, the invention provides being used for calibrating the nano particle size standard substance of granulometry,
It is made up of the spheroidal particle for 80-600nm for the nominal particle size, spheroidal particle is spherical.Nominal particle size refers to manage
By the diameter that above should reach.
According to the embodiment of the present invention, above-mentioned nano particle size standard substance is made by step as shown in Figure 1：Prepare
Step S110：Tetraethyl orthosilicate and ethanol are added in reactor, mixes, and distilled water and ammonia are stirred formation mixing
Liquid；Reactions steps S120：Mixed liquor is slowly instilled in reactor, continuously stirred, completion of dropping, continue to stir at a predetermined temperature
Mix the scheduled time, obtain spherical emulsion；With cleaning step S130：Deionized water eccentric cleaning silicon dioxide
Spheroidal particle emulsion, obtains spherical.
According to the embodiment of the present invention, the tetraethyl orthosilicate in preparation process can be 5-10mL, and ethanol can be
100-150mL, distilled water can be 5-30mL, and ammonia can be 10-15mL.
According to the embodiment of the present invention, the stir speed (S.S.) in reactions steps can be 200-400r/min, drop rate
Can be 0.1-0.5mL/s.
According to the embodiment of the present invention, the predetermined temperature in reactions steps can be 25-35 DEG C, and the scheduled time can be
3h.
According to the embodiment of the present invention, the centrifugation in cleaning step can be under centrifugation rate be for 6000-9000r/min
Carry out 8-15min.
According to the embodiment of the present invention, above-mentioned nano particle size standard substance further by microscopic method come definite value, its
In, comprised the steps come definite value by microscopic method：Using scanning electron microscope to certain amount of spherical crosslinking polyphenyl
Ethylene standard particle is amplified, and shoots the image of spherical crosslinked polystyrene standard particle one by one；In same amplification
The area to determine single pixel under amplification for the scale of lower determination standard micrometer；By calculating the picture that standard particle comprises
The quantity of element, determines the equivalent projected area of standard particle, thus obtaining the equivalent diameter projected of standard particle；Measure every one by one
The particle diameter of individual standard particle, to carry out definite value.
According to another implementation of the invention, the present invention provides one kind as shown in Figure 1 to be used for calibrating granulometry
Nano particle size standard substance preparation method, comprise the following steps：Preparation process S110：Tetraethyl orthosilicate and ethanol are added
In reactor, mix, and distilled water and ammonia are stirred formation mixed liquor；Reactions steps S120：Mixed liquor is slowly dripped
Enter in reactor, continuously stirred, completion of dropping, continues to stir the scheduled time at a predetermined temperature, obtains spherical of silicon dioxide
Grain emulsion；With cleaning step S130：Deionized water eccentric cleaning spherical emulsion, obtains silicon dioxide spherical
Granule.
According to another implementation of the invention, above-mentioned preparation method also includes the step by microscopic method come definite value
Suddenly, wherein, comprised the steps come definite value by microscopic method：Using scanning electron microscope to certain amount of spherical crosslinking
Polystyrene standard granule is amplified, and shoots the image of spherical crosslinked polystyrene standard particle one by one；In same amplification
The area to determine single pixel under amplification for the scale of determination standard micrometer under multiple；Comprised by calculating standard particle
Pixel quantity, determine the equivalent projected area of standard particle, thus obtaining the equivalent diameter projected of standard particle；Survey one by one
Measure the particle diameter of each standard particle, to carry out definite value.
The uncertainty of following embodiment Plays material definite values includes：The measurement of the inaccurate introducing of micrometer does not know
Degree；The uncertainty of measurement introducing when being calibrated using micrometer；The measurement of certain granule introducing is continuously measured not after calibration
Degree of certainty；The uncertainty of measurement four part composition of the uneven and unstable introducing of standard substance.The uncertainty result being given
Overall uncertainty for four part uncertainty combinations.
Embodiment 1, nominal particle size are the preparation of the silica dioxide granule of 80nm
Nominal particle size is the silica dioxide granule of 80nm, is made by following steps：
Preparation process：5mL tetraethyl orthosilicate and 150mL ethanol are added in reactor, mixes, and take 5mL water and 15mL
Ammonia stirs formation mixed liquor；
Reactions steps：Mixed liquor is instilled in reactor with the drop rate of 0.2mL/s, and persistently stirs under 300r/min
Mix, completion of dropping, continue stirring 3 hours at 25 DEG C, obtain spherical emulsion；Cleaning step：Using go from
Sub- water eccentric cleaning, centrifugation rate is 6000r/min, and the time is 15in, obtains spherical.Obtained 80nm
Spherical as shown in Fig. 2 as seen from the figure, spherical manufactured in the present embodiment is uniform in size,
Smooth surface, no damaged, zero defect, monodispersity is good.
Using method of analysis of variance (F analytic process) and meansigma methodss consistency-checking method (t method of inspection) inspection the present embodiment preparation
The uniformity of spherical and stability it was demonstrated that its uniformity and having good stability.
Definite value is carried out to spherical manufactured in the present embodiment by microscopic method, comprises the steps：Adopt
With scanning electron microscope, certain amount of spherical crosslinked polystyrene standard particle is amplified, and shoots spherical friendship one by one
The image of polystyrene standard particle；Determine the scale of standard micrometer to determine under amplification under same amplification
The area of single pixel；By calculating the quantity of the pixel that standard particle comprises, determine the equivalent projected area of standard particle, from
And obtain the equivalent diameter projected of standard particle；Measure the particle diameter of each standard particle one by one, to carry out definite value.Definite value result is
Number average particle size is 79nm, and uncertainty is ± 0.64nm.
Embodiment 2, nominal particle size are the preparation of the silica dioxide granule of 80nm
Nominal particle size is the silica dioxide granule of 80nm, is made by following steps：
Preparation process：10mL tetraethyl orthosilicate and 100mL ethanol are added in reactor, mix, and take 30mL water and
10mL ammonia stirs formation mixed liquor；
Reactions steps：Mixed liquor is instilled in reactor with the drop rate of 0.1mL/s, and persistently stirs under 200r/min
Mix, completion of dropping, continue stirring 3 hours at 35 DEG C, obtain spherical emulsion；Cleaning step：Using go from
Sub- water eccentric cleaning, centrifugation rate is 9000r/min, and the time is 8min, obtains the silicon dioxide that nominal particle size is 80nm spherical
Granule.
Using method of analysis of variance (F analytic process) and meansigma methodss consistency-checking method (t method of inspection) inspection the present embodiment preparation
The uniformity of spherical and stability it was demonstrated that its uniformity and having good stability.
Definite value is carried out to spherical manufactured in the present embodiment by microscopic method, comprises the steps：Adopt
With scanning electron microscope, certain amount of spherical crosslinked polystyrene standard particle is amplified, and shoots spherical friendship one by one
The image of polystyrene standard particle；Determine the scale of standard micrometer to determine under amplification under same amplification
The area of single pixel；By calculating the quantity of the pixel that standard particle comprises, determine the equivalent projected area of standard particle, from
And obtain the equivalent diameter projected of standard particle；Measure the particle diameter of each standard particle one by one, to carry out definite value.Definite value result is
Number average particle size is 81nm, and uncertainty is ± 0.92nm.
Embodiment 3, nominal particle size are the preparation of the silica dioxide granule of 80nm
Nominal particle size is the silica dioxide granule of 80nm, is made by following steps：
Preparation process：8mL tetraethyl orthosilicate and 120mL ethanol are added in reactor, mixes, and take 15mL water and 12mL
Ammonia stirs formation mixed liquor；
Reactions steps：Mixed liquor is instilled in reactor with the drop rate of 0.5mL/s, and persistently stirs under 400r/min
Mix, completion of dropping, continue stirring 3 hours at 30 DEG C, obtain spherical emulsion；Cleaning step：Using go from
Sub- water eccentric cleaning, centrifugation rate is 8000r/min, and the time is 10min, obtains the silicon dioxide that nominal particle size is 80nm spherical
Granule.
Using method of analysis of variance (F analytic process) and meansigma methodss consistency-checking method (t method of inspection) inspection the present embodiment preparation
The uniformity of spherical and stability it was demonstrated that its uniformity and having good stability.
Definite value is carried out to spherical manufactured in the present embodiment by microscopic method, comprises the steps：Adopt
With scanning electron microscope, certain amount of spherical crosslinked polystyrene standard particle is amplified, and shoots spherical friendship one by one
The image of polystyrene standard particle；Determine the scale of standard micrometer to determine under amplification under same amplification
The area of single pixel；By calculating the quantity of the pixel that standard particle comprises, determine the equivalent projected area of standard particle, from
And obtain the equivalent diameter projected of standard particle；Measure the particle diameter of each standard particle one by one, to carry out definite value.Definite value result is
Number average particle size is 82nm, and uncertainty is ± 0.79nm.
Embodiment 4, nominal particle size are the preparation of the silica dioxide granule of 300nm
Nominal particle size is the silica dioxide granule of 300nm, is made by following steps：
Preparation process：5mL tetraethyl orthosilicate and 120mL ethanol are added in reactor, mixes, and take 15mL water and 10mL
Ammonia stirs formation mixed liquor；
Reactions steps：Mixed liquor is instilled in reactor with the drop rate of 0.4mL/s, and persistently stirs under 400r/min
Mix, completion of dropping, continue stirring 3 hours at 30 DEG C, obtain spherical emulsion；Cleaning step：Using go from
Sub- water eccentric cleaning, centrifugation rate is 9000r/min, and the time is 8min, obtains the silicon dioxide that nominal particle size is 300nm spherical
Granule.The spherical of obtained 300nm as shown in figure 3, as seen from the figure, silicon dioxide manufactured in the present embodiment
Spheroidal particle is uniform in size, smooth surface, no damaged, zero defect, and monodispersity is good.
Using method of analysis of variance (F analytic process) and meansigma methodss consistency-checking method (t method of inspection) inspection the present embodiment preparation
The uniformity of spherical and stability it was demonstrated that its uniformity and having good stability.
Definite value is carried out to spherical manufactured in the present embodiment by microscopic method, comprises the steps：Adopt
With scanning electron microscope, certain amount of spherical crosslinked polystyrene standard particle is amplified, and shoots spherical friendship one by one
The image of polystyrene standard particle；Determine the scale of standard micrometer to determine under amplification under same amplification
The area of single pixel；By calculating the quantity of the pixel that standard particle comprises, determine the equivalent projected area of standard particle, from
And obtain the equivalent diameter projected of standard particle；Measure the particle diameter of each standard particle one by one, to carry out definite value.Definite value result is
Number average particle size is 312nm, and uncertainty is ± 1.02nm.
Embodiment 5, nominal particle size are the preparation of the silica dioxide granule of 600nm
Nominal particle size is the silica dioxide granule of 600nm, is made by following steps：
Preparation process：10mL tetraethyl orthosilicate and 100mL ethanol are added in reactor, mix, and take 25mL water and
13mL ammonia stirs formation mixed liquor；
Reactions steps：Mixed liquor is instilled in reactor with the drop rate of 0.5mL/s, and persistently stirs under 200r/min
Mix, completion of dropping, continue stirring 3 hours at 30 DEG C, obtain spherical emulsion；Cleaning step：Using go from
Sub- water eccentric cleaning, centrifugation rate is 7000r/min, and the time is 9min, obtains the silicon dioxide that nominal particle size is 600nm spherical
Granule.The spherical of obtained 600nm as shown in figure 4, as seen from the figure, silicon dioxide manufactured in the present embodiment
Spheroidal particle is uniform in size, smooth surface, no damaged, zero defect, and monodispersity is good.
Using method of analysis of variance (F analytic process) and meansigma methodss consistency-checking method (t method of inspection) inspection the present embodiment preparation
The uniformity of spherical and stability it was demonstrated that its uniformity and having good stability.
Definite value is carried out to spherical manufactured in the present embodiment by microscopic method, comprises the steps：Adopt
With scanning electron microscope, certain amount of spherical crosslinked polystyrene standard particle is amplified, and shoots spherical friendship one by one
The image of polystyrene standard particle；Determine the scale of standard micrometer to determine under amplification under same amplification
The area of single pixel；By calculating the quantity of the pixel that standard particle comprises, determine the equivalent projected area of standard particle, from
And obtain the equivalent diameter projected of standard particle；Measure the particle diameter of each standard particle one by one, to carry out definite value.Definite value result is
Number average particle size is 592nm, and uncertainty is ± 0.88nm.
In sum, the nano particle size standard substance of present invention preparation can reach national standard reference material requirement, and
And disclosure satisfy that the calibration requirements of particle sizing.
Embodiments above is only used for that the present invention will be further described it is impossible to be interpreted as to the scope of the present invention
Limit.Any engineers and technicians being familiar with this field the present invention is done according to foregoing invention content some nonessential change
Enter and adjust, all should be included within the scope of the present invention.
Claims (9)
1. it is used for calibrating the nano particle size standard substance of granulometry, be made up of the spheroidal particle for 80-600nm for the nominal particle size,
Described spheroidal particle is spherical.
2. nano particle size standard substance according to claim 1, it makes as follows：
Preparation process：Tetraethyl orthosilicate and ethanol are added in reactor, mixes, and distilled water and ammonia are stirred formed
Mixed liquor；
Reactions steps：Described mixed liquor is slowly instilled in described reactor, continuously stirred, completion of dropping, continues in pre- constant temperature
Degree is lower to stir the scheduled time, obtains spherical emulsion；With
Cleaning step：Spherical emulsion described in deionized water eccentric cleaning, obtains described silicon dioxide spherical
Granule.
3. nano particle size standard substance according to claim 2, wherein, the tetraethyl orthosilicate in described preparation process is 5-
10mL, ethanol is 100-150mL, and distilled water is 5-30mL, and ammonia is 10-15mL.
4. nano particle size standard substance according to claim 2, wherein, the stir speed (S.S.) in described reactions steps is 200-
400r/min, drop rate is 0.1-0.5mL/s.
5. nano particle size standard substance according to claim 2, wherein, the predetermined temperature in described reactions steps is 25-
35 DEG C, the scheduled time is 3h.
6. nano particle size standard substance according to claim 2, wherein, the centrifugation in described cleaning step is in centrifugation rate
For carrying out 8-15min under 6000-9000r/min.
7. the nano particle size standard substance according to claim 2-6, its further by microscopic method come definite value, its
In, described comprised the steps come definite value by microscopic method：
Using scanning electron microscope, certain amount of described spherical crosslinked polystyrene standard particle is amplified, and one by one
Shoot the image of described spherical crosslinked polystyrene standard particle；
The area to determine single pixel under described amplification for the scale of determination standard micrometer under same amplification；
By calculating the quantity of the pixel that described standard particle comprises, determine the equivalent projected area of described standard particle, thus
Obtain the equivalent diameter projected of described standard particle；
Measure the particle diameter of each described standard particle one by one, to carry out definite value.
8. a kind of preparation method of the nano particle size standard substance for calibrating granulometry, comprises the following steps：
Preparation process：Tetraethyl orthosilicate and ethanol are added in reactor, mixes, and distilled water and ammonia are stirred formed
Mixed liquor；
Reactions steps：Described mixed liquor is slowly instilled in described reactor, continuously stirred, completion of dropping, continues in pre- constant temperature
Degree is lower to stir the scheduled time, obtains spherical emulsion；With
Cleaning step：Spherical emulsion described in deionized water eccentric cleaning, obtains described silicon dioxide spherical
Granule.
9. preparation method according to claim 8, also includes the step come definite value by microscopic method, wherein, described logical
Cross microscopic method and carry out definite value and comprise the steps：
Using scanning electron microscope, certain amount of described spherical crosslinked polystyrene standard particle is amplified, and one by one
Shoot the image of described spherical crosslinked polystyrene standard particle；
The area to determine single pixel under described amplification for the scale of determination standard micrometer under same amplification；
By calculating the quantity of the pixel that described standard particle comprises, determine the equivalent projected area of described standard particle, thus
Obtain the equivalent diameter projected of described standard particle；
Measure the particle diameter of each described standard particle one by one, to carry out definite value.
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| CN116199208A (en) * | 2023-03-02 | 2023-06-02 | 四川大学 | Preparation of conductive nano carbon sphere and calibration application of conductive nano carbon sphere in scanning electron microscope |
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| CN101891208A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing submicron silicon dioxide spherical particles |
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| CN101891208A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing submicron silicon dioxide spherical particles |
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