CN103760074B - The Particle Size Determination Method of the irregular powder body material of particle morphology - Google Patents
The Particle Size Determination Method of the irregular powder body material of particle morphology Download PDFInfo
- Publication number
- CN103760074B CN103760074B CN201410015067.2A CN201410015067A CN103760074B CN 103760074 B CN103760074 B CN 103760074B CN 201410015067 A CN201410015067 A CN 201410015067A CN 103760074 B CN103760074 B CN 103760074B
- Authority
- CN
- China
- Prior art keywords
- particle
- powder body
- body material
- particle size
- determination method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention belongs to the detection technique of powder body material, be specifically related to the Particle Size Determination Method of a kind of irregular powder body material of particle morphology being applied to pulpous state system.Process for dispersing when this powder body material downstream user of irregular for particle morphology powder body material sampling simulation is used by it makes scattered slurry；The suspension of low concentration is made after taking pulp-like dilution and disperseing further with ultrasound wave；Take hanging drop be added to band support film transmission electron microscope special purpose copper online；Observe with high magnification after first observing dispersion situation under low range after copper mesh is put into transmission electron microscope and take pictures；To the particle measurement maximum gauge in photo and minimum diameter, and carry out by stages statistical analysis according to maximum particle diameter.The method according to the invention convenient can accurately reflect out particle morphology irregular powder body material application effect in downstream user.
Description
Technical field
The invention belongs to the detection technique of powder body material, be specifically related to a kind of be applied to the particle morphology of pulpous state system not
The Particle Size Determination Method of the powder body material of rule.
Background technology
For powder body material, it is spheroidal particle that most downstream application field is intended to its pattern, but the biggest
Part powder body material particle morphology is the most irregular, its shape have needle-like, horn shape, dendroid, threadiness,
Lamellar, granular warty etc..For its diversified particle morphology, for convenience of measuring and statement, the most all roots
According to geometry, kinetics, optical characteristics etc. such as the projected area of particle, volume, sedimentation velocity by the pattern of particle
Equivalence globulate measures particle diameter, and statement particle diameter is straight with equivalent perimeter diameter, equivalent area diameter and equivalent volume
Footpath etc..Typical assay method has sieve method, centrifugal liquid phase sedimentation, resistance actinobolia, laser diffractometry, electricity
Sub-microscopic method.Being generally used for measuring the powder body material that particle diameter is thicker for sieve method, the scope of application is the least.Centrifugal
The particle size range that liquid deposition method, resistance actinobolia, laser diffractometry etc. can be measured is wider, typically uses ultrasound wave
Dispersion machine is dispersed into slurry under the conditions of same and measures, but the pole of the irregular powder body material of particle morphology own
Easily occur to flocculate and reunite, scattered slurry inevitably exists many floccule bodys and aggregate, is dividing
In the case of bulk condition does not measures, these measuring methods are manually set scope the most in advance, by the most scattered wadding
Solidifying body and aggregate are ignored, and the result often recorded is pattern rule relatively, the particle diameter of easy divided particles,
The result so recorded has bigger deviation with the particle situation of powder body material itself.Sink additionally for centrifugal liquid phase
Fall method, resistance actinobolia, laser diffractometry etc. are used for detecting powder body material, and sampling amount seldom (typically takes
Sample amount is less than 1g), the most inadequate for industrialized its samples' representativeness of powder body material product.For routine
The particle diameter of electron microscope method detection powder body material, sampling amount during detection is usually no more than 0.1g, the speed of detection
Slowly, the particle diameter and the pattern that are mainly used in the lab scale sample of scientific research institutions measure, the grain measured according to sem image
The data that footpath is selected also are not quite similar, and the Accurate Determining for the particle diameter of industrialization powder body material product is relatively difficult.
The current mensuration at industrialization powder body material product cut size is widely used mainly centrifugal liquid phase sedimentation and laser
Diffraction approach, wherein laser diffractometry is owing to it is convenient and swift and is suitable for the big characteristic of particle size range in producing reality
Most widely used.
Laser diffractometry is that the largest light intensity angle of diffraction according to granule measures particle diameter with the principle that its particle diameter is inversely proportional to,
Its result is independent of the number of particle, generally uses percent by volume to represent its measurement result, represents with D [4,3].
The frequency of appearance is added up respectively in the interval that concrete grain size distribution uses instrument to delimit according to its mathematical model then
Being depicted as scattergram and calculate D50, D10, D90 etc., from the point of view of actually used situation, instrument is to each
The delimitation of particle size interval is change, and general calculating does not go out the content of the particle of theory or actual true needs part,
For the particle content of (half-wavelength of visible ray, 200～350nm) in the ideal size range required for titanium dioxide
Cannot calculate.For its measuring principle, the accuracy of measurement result depends on the light of tested powder body material
Learn parameter (refractive index), the surface topography defect of powder body material, lattice defect to the absorption of laser, reflect, spread out
Penetrate the difference of effect, and single-particle etc. can be dispersed into the most every time.On the other hand, though the surface of its particle
In the case of situation is the most consistent with dispersion situation, owing to its typical particle diameter statistical method is 6 times to diameter of light intensity
The mathematical model of side converts, thus more ignores the impact of small particles, is exaggerated the impact of big particle.For
For the application of powder body material, we more use the grain effect of its single particle, such as pigment particles application
Coating system is wished each meet to optical effect require number of particles The more the better, less than theoretical or actual
Require that the particle of particle diameter is inoperative, the most only just correspond to single target more than each particle of target grain size requirement and want
Ask the effect of particle.Therefore, the particle diameter of the laser diffractometry powder body material for measuring is answered to be characterized in downstream
Bigger defect is there is by the application effect in field.
The advantage of electron microscope method is to see the pattern of powder body material granule, but due to its sample preparation difficulty, cost
High, detection speed slowly, thus is mainly used in scientific research, industrial little employing.Electron microscope method is by powder body material
Expecting that scattered rear sample preparation is observed, carry out statistical analysis according to the still image observed and calculate particle diameter, it is typical
Advantage is to see the pattern of particle.For electron microscope method, no matter use transmission electron microscope (TEM)
Or scanning electron microscope (SEM) measures particle diameter, all sample preparation is required the highest.If powder body material does not has
Have fully dispersed come or repeatedly drip during net processed all can cause particle flocculation on sample stage (such as copper mesh) and many
Layer stack is amassed, even if the still image made can tell the size of each granule, and also can be to follow-up grain diameter measurement band
Carry out huge trouble, have a strong impact on measurement efficiency.According to measuring and calculating, a skilled person general for this still image
Within one day, also it is only capable of measuring about 2000 particles.The powder body of Gauss distribution is met generally, for particle diameter distribution
The mass median particle diameter of the material error to be obtained powder body material within 5% needs the number of about 61000 particles
According to, and the particle diameter of the irregular powder body material of most of particle morphology is distributed and does not meets Gauss distribution, therefore need system
The number of particles of meter also runs far deeper than aforesaid quantity.Therefore, the finding speed of electron microscope method is the slowest.
Summary of the invention
Problem to be solved by this invention is to provide a kind of behaviour using determination of electron microscopy to be applied to pulpous state system
Make easy, the side of the high particle morphology irregular powder body material particle diameter good with the downstream application goodness of fit of detection efficiency
Method, it comprises the steps of
A: the powder body material insoluble in solvent is joined and makes the slurry that mass concentration is 20～70% in solvent,
Add powder quality 1～the dispersant of 10%, and the abrasive media of 0.8～3 times of quality of total stock quality uses and shakes
Swing mill or sand mill is ground dispersion and processes；Measuring fineness less than 5 microns with Hegman grind gage is dispersion terminal；
Described powder body can be titanium dioxide, and solvent is dehydrated alcohol, is separated into Bi Ke company BYK111, this company of hamming
NUOSPERSE FA196 or three kinds of dispersants of polyvinylpyrrolidone in one；
B: the slurry taking the acquisition of step A adds the suspension that solvent dilution becomes concentration to be 0.2～2.5%, uses ultrasound wave
Disperse 1～10 minute；
C: take the hanging drop described in step B with micropipettor or capillary tube and be added to the transmission electron microscope of band support film
(TEM) special purpose copper is online, makes particle tile on copper mesh and uses transmission electron microscope (TEM) to see after drying
Survey and make photo；
D: use craft or the maximum gauge (Dmax) of software measurement 1000～10000 particles and minimum diameter
(Dmin), then statistics particle diameter is distributed and particle morphology.
Preferably, for making powder body material sampling have more representativeness in above-mentioned steps A, for vibration mill dispersion,
The sampling amount of powder body material is not less than 5g, and the scattered sampling amount of sand mill is not less than 50g.
Preferably, above-mentioned steps A is less than for oil absorption the powder body of 30g/100g, grinds concentration and select
40～65%, dispersant dosage is the 1～5% of powder quality；For the oil absorption powder body more than 30g/100g, grind
Concentration selects 30～50%, and dispersant dosage is the 2～10% of powder quality.
Preferably, in above-mentioned steps A, abrasive media uses zirconium pearl, and zirconium pearl selects a diameter of 0.4～0.6,
0.6～0.8mm, 0.8～1.0mm, 1.0mm～1.2mm, 1.2mm～1.4mm, 1.4～1.6mm, 1.6～1.8mm,
Zirconium pearl is used in the grinding of 1.8～2.0mm specifications.
Preferably, the addition of abrasive media in above-mentioned steps A, for vibration mill dispersion, adding of abrasive media
Enter amount and total stock quality than for 0.8:1～2:1；Sand milling is disperseed, the addition of abrasive media and total stock quality
Ratio is 1:1～3:1.
Preferably, in above-mentioned steps A, the judgement of grinding distribution terminal uses Hegman grind gage to measure, fineness of dispersion
Less than 5 microns, and on Hegman grind gage, under 5 micron scale, visible particle number is not more than 50.
Preferably for the powder body that mean diameter is 0.01～0.8 micron in step B, diluted concentration is selected
0.2～1.2%；0.8～2.0% is selected for the mean diameter powder body diluted concentration more than 0.8 micron.
Preferably, in above-mentioned steps C, the volume of the suspension that micropipettor or capillary tube pipette is 5～15 microlitres,
It is that disposable dropping 1～2 drips to tile on the net with the TEM special purpose copper thick less than 20nm when being added drop-wise to copper mesh
It is dried.Use and support that the film thickness copper mesh less than 20nm is conducive to making the electromicroscopic photograph that black and white contrast is strong, from
And the convenient artificial or measurement statistics of software.
Preferably, the transmission electron microscope in above-mentioned steps C (TEM) need to use the standard grain of known particle diameter
The scale (scale) of son correction TEM.
Preferably, when above-mentioned steps C uses transmission electron microscope (TEM) observation, first see by low range
Survey the particle within the vision dispersion situation of each diameter 40 microns, amplify the multiplying power of TEM, make visual field model
Enclosing interior number of particles is 10～60, fixed multiplying power, takes pictures for detection particle diameter after focusing.It is right to need when detection is taken pictures
Particle in each visual field of 40 microns all and is not repeatedly taken pictures, to ensure the accurate of testing result
Property also reduces amount detection.
The measuring method of described maximum gauge and minimum diameter is: find on particle shape projection line the two of furthest apart
Individual, A and B, and it is linked to be a line segment AB；Drawing circle with AB for diameter, this circle will project with particle shape
A, B on line 2 is tangent, checks whether A, B 2 is 2 farthest points, if it is, A, B two
The distance of point is maximum gauge (Dmax)；Drawing straight line, the midpoint of this straight-line pass AB is also perpendicular to AB,
Intersecting at E and F with particle shape projection line, the distance that E, F are 2 is minimum diameter (Dmin).
The particle diameter that in described step D, the statistics of particle diameter distribution uses is maximum gauge (Dmax).
In described step D, particle morphology uses form factor F value to represent, i.e. each particle is used minimum diameter
(Dmin) volume that spheroid calculates and the ratio of volume that maximum gauge (Dmax) is calculated are pressed by spheroid.F value
The biggest, then particle is closer to spherical.
In described step D, the statistics of particle diameter distribution and particle morphology uses point three intervals to add up respectively, i.e.
Statistics coincidence theory and or the particle size range of actual requirement in number of particles after calculate hundred shared by this number of particles
Divide content, and calculate the arithmetic mean of instantaneous value of this scope particle F value；Statistics is less than theoretical and or the particle diameter of actual requirement
Calculate the percentage composition shared by this number of particles after the number of particles of scope, and calculate the arithmetic of this scope particle F value
Meansigma methods；And statistics more than theoretical and or actual requirement particle size range number of particles after calculate this number of particles
Shared percentage composition, and calculate the arithmetic mean of instantaneous value of this scope particle F value.
Electron microscope method can be applied to the quality control of industrialization powder body material by the present invention and application performance is commented
Valency, its use uses the corresponding process for dispersing of process for dispersing during this product to disperse, at particle with downstream user
In the case of lacking overlap as far as possible during fully dispersed and sample preparation, can obtain accurately by reducing the number of measurement particle
Testing result improves detection efficiency, obtains black and white contrast additionally by the means such as accelerating potential adjusting Electronic Speculum strong
Electromicroscopic photograph, thus use that electron microscope method is also comparable to be measured particle diameter quickly and easily and can give play to electronics
Microscopic method can observe the advantage of each particle morphology.Its measurement result is actually used with downstream application field simultaneously
Effect is consistent.
Detailed description of the invention
Described in further detail to the present invention below by specific embodiment.
Embodiment 1
(1) preparation of samples:
Sample A: import sulfuric acid process Rutile type titanium dioxide (trade mark is RDI-S), is mainly used in high-grade ink,
Industrial paint.
Sample B: import chloride process rutile type titanium dioxide (trade mark is Tiona 595), is mainly used in paint, is coated with
Material.
Sample C: domestic outstanding sulfuric acid process Rutile type titanium dioxide (trade mark is SR-9000), is mainly used in oil
Ink, paint and coating.
The sulfuric acid process Rutile type titanium dioxide of sample D: domestic routine, is mainly used in paint, coating.
(2) grinding distribution
Taking 4 volumes is the vial of 50ml, is separately added into the zirconium pearl 40g of a diameter of 1.0～1.2mm, anhydrous
Ethanol 12g and 0.12gBYK111 dispersant, weigh four each 10g of sample the most respectively and add in vial,
Put into after vial is sealed in vibration mill and disperse.Consisting of of its abrasive final: powder body material 10g；Grind
Stock quality concentration is 45.5%；Dispersant addition is 1.2%；Zirconium pearl amount is 1.8:1 with the ratio of ground slurry.
Vibrating dispersion samples detection once in after 20 minutes every 5 minutes, takes as Hegman fineness grind reaches less than 5 microns these samples
Going out, sampling dehydrated alcohol was diluted to the concentration of 1.0% immediately after, with ultrasonic disperse 3 minutes.Vibrating dispersion institute
Take time as sample A:35 minute；Sample B:35 minute；Sample C:40 minute；Sample D:60 minute.
(3) sample preparation
Under ultrasound wave dispersity, take suspension with the capillary tube of internal diameter 0.5mm, then drip suspension extremely
Support on the copper mesh of film with 10nm carbon, natural drying.
(4) detect and add up
The logical net the made dispersion situation that low multiple observes on TEM.On TEM, high multiple observes
For particle size determination and the representative pictures of evaluation powder body material particle diameter.The particle diameter distribution statistics of sample and shape because of
Number is shown in Table 1.
The particle diameter distribution statistics table of table 1 sample and pattern statistics
In upper table, volume average particle size formula is as follows:
Volume average particle size
(5) particle diameter distribution and particle morphology statistical result are corresponding with downstream application effect
Titanium dioxide is a kind of the most widely used Chinese white, has the highest refractive index in Chinese white.Right
Target is controlled: for making the refractive index of titanium dioxide in the titanium dioxide well-known particle diameter of industry technology personnel and particle morphology
Be able to the highest presenting, it is thus achieved that the highest light scattering ability thus reach more preferable covering power and present good white
Color, the titanium dioxide particle of production it would be desirable that particle diameter is the visible ray light wave of 400～700nm (wavelength be) wavelength
The spheroidal particle content of the half of scope is the most, i.e. diameter control 200～350nm spheroidal particle number want
The most.If the particle diameter of titanium dioxide is the highest at the content of 200～350nm parts, the highest then covering power of sphericity
The highest.It addition, corase particles content is the highest in titanium dioxide, i.e. the highest more than the particle content of 350nm part, then make
The goods glossiness made with titanium dioxide is the poorest.
From in table 1:
For covering power:
Sample A particle diameter particle content in 200～350nm intervals reaches 53.0%, for the highest, thus has
The highest covering power；The particle diameter of sample B and C particle content in the range of 200～350nm is respectively 43.6%
With 43.8%, almost equal, but the arithmetic mean of instantaneous value of this particle size interval sphericity is respectively 0.265 and 0.231, sample
The F value of product B is the highest, and therefore the covering power of sample B is higher than sample C；Sample D particle diameter is 200～350nm
In the range of particle content be 40.4%, for minimum, the arithmetic mean of instantaneous value of this particle size interval F value is 0.213, F value
Also minimum, therefore covering power is minimum.
For gloss:
The percentage composition of the granule number that sample A, B, C, D particle diameter is interval more than 350nm is respectively 10.6%,
11.2%, 12.1% and 16.4%, gloss order from high in the end is sample A > sample B > sample C > sample D.
The result of above-mentioned covering power and gloss and titanium dioxide industry and the cognitive result of downstream application industry technology personnel
Completely the same, i.e. sample A (trade mark is RDI-S) is that the whole world is famous has brilliance for ink, paint industry
Covering power and the product of gloss；Sample B (trade mark is Tiona 595) famous is used for painting for the whole world, coating
The high covering power of industry and the product of gloss；Sample C (trade mark is SR-9000) is domestic outstanding product, main
It is used for paint and ink；Sample D is the product of domestic regular quality level, is common to various paint, coating.
Tetra-samples of sample A, B, C, D are carried out application test detection and verifies particle diameter distribution and particle morphology system
The accuracy of meter result.Table 2 is applying detection result.
Table 2 applying detection result
In table 2, covering power and gloss in acrylic paint use following methods to detect:
Adding 100g bead in 200ml vial, (resin solid content is 50g thermoplastic propene's acid solution
33%) and 10.8g titanium dioxide sample, after sealing, on vibration mill, grinding distribution to scraper plate is read in detail and is reached 10 microns,
Make the paint that pigment volume concentration (PVC) is 20%.Then take 5g and paint the bar spreader with 60 microns at black and white card
Carry out film on paper, for ensureing the accuracy of result, be coated with membrane process and use automatic film applicator film.Natural drying 24
After hour, measure the contrast ratio of film (paint film).The mensuration of paint film contrast ratio is according to GB/T 13452.3-1992
" Part I that measures of paint and varnish covering power is suitable to the Kubelka-Munk method of white and light colour paint " enters
Row measures.
Result verification from Tables 1 and 2 goes out particle diameter between titanium dioxide theory and or the particle size range of actual requirement
The highest then covering power of number of particles percentage ratio of (200～350nm) is the highest, and F value more high covering power is the highest；Greatly
The highest then glossiness of percentage composition in 350nm granule number is the poorest.
It is emphasized that volume mean diameter D [4,3] is to calculate according to the computational methods of laser particle analyzer in table 1
The particle diameter gone out, invents for edition with parallel text, does not the most substantially exist with downstream application effect and significantly associate
Property.
Embodiment 2
(1) preparation of samples:
Sample E: import blanc fixe (trade mark is Blanc Fixe Micro), is mainly used in the industry such as automobile coating
Paint.
Sample F: domestic blanc fixe (place of production is Hunan), is mainly used in paint, coating etc..
(2) grinding distribution
Try to please and amass the rustless steel drum with cooling jacket into 500ml, add 300g a diameter of 0.6～0.8mm
Zirconium pearl, 120g dehydrated alcohol and 3.6g polyvinylpyrrolidone dispersant, after having weighed by rustless steel circle
Bucket is put to sand mill, connects cooling water, opens sand mill, and rotating speed is adjusted to 800r/min, then at this stirring shape
120g sample E is added under state.Add after sample E continues stirring 5 minutes and rotating speed is risen to 3000r/min sand milling also
Start timing.Consisting of of its abrasive final: powder body material 120g；Ground slurry mass concentration is 50%；Point
Powder addition is 3%；Zirconium pearl amount is 1.25:1 with the ratio of ground slurry.Sampling is not stopped with scraping in sand grinding process
Plate fineness gauge measures Hegman fineness grind, reaches less than 5 microns stopping sand millings such as Hegman fineness grind and anhydrous second is used in sampling immediately
Alcohol was diluted to the concentration of 1.5%, with ultrasonic disperse 3 minutes.Sample F is processed by same process.Final sand milling divides
Scattered required time is: sample E, 25 minutes；Sample F, 30 minutes.
(3) sample preparation
Disperse ceaselessly to take suspension with the micropipettor that range is 10 microlitres under situation at ultrasound wave, then drip
A droplet suspension is extremely supported on the copper mesh of film with 15nm carbon, natural drying.
(4) detect and add up
The particle diameter distribution statistics of sample and form factor are shown in Table 3.
The particle diameter distribution statistics table of table 3 sample and pattern statistics
In upper table, volume average particle size formula is as follows:
Volume average particle size
(5) particle diameter distribution and particle morphology statistical result are corresponding with downstream application effect
Blanc fixe is the outstanding filler of a kind of stable chemical nature safety non-toxic, be widely used in paint, plastics,
The industries such as papermaking, in various fillers, the refractive index of blanc fixe is the highest, reaches 1.64, has certain covering
Power.Industrialized blanc fixe owing to using double decomposition precipitation method to produce when it produces and precipitation is rapid, because of
And particle diameter wider distribution, often use as a kind of simple filler.But the precipitated sulfur through good size controlling
Acid barium can accomplish that the particle diameter of the predecessor with titanium dioxide is closer to, in color stuffing dispersion, to titanium dioxide
All there is certain steric hindrance in particle, is on the one hand conducive to the uniform diffusion of titanium dioxide particle, on the other hand can hinder
Hinder the Collision coagulation of titanium dioxide particle, it is thus possible to promote the interval dispersion of titanium dioxide particle and improve titanium dioxide particle
Stably dispersing performance.(such as industrial paints system) in the mixed system of a blanc fixe and titanium dioxide, right
In having the blanc fixe similar to the particle diameter of titanium dioxide predecessor, from embodiment 1, particle diameter exists
In the range of 200～350nm, the content high energy of particle presents good white and covering power, therefore blanc fixe particle
Particle diameter number of particles content in the range of 200～350nm the highest, the most more can give full play to its high index
Characteristic, can obtain certain covering power, and titanium dioxide particle can be formed significant interval as previously mentioned, improve titanium
The efficiency of white lead particle, the effect of these two aspects, the ratio system individually with the titanium dioxide of equivalent can be obtained higher
Covering power.Thus can be with a part of this blanc fixe replacement titanium dioxide similar with titanium dioxide particle diameter
Not reducing covering power, this blanc fixe is in print with the name sale of a kind of pigment interval dose.Thus, may be used
To find out the blanc fixe as pigment interval dose, coincidence theory and or the particle size range of actual requirement be
200～350nm.It addition, the glossiness being more than the coarse granule manufactured goods the most at most of 350nm is the poorest.For particle shape
For looks, form factor F value is the biggest, and to be i.e. closer to spherical then interval action the biggest.
From in table 3:
For covering power:
Sample E particle diameter particle content in the range of 200～350nm reaches 44.1%, and the arithmetic mean of instantaneous value of F value is
0.322, will be high relative to the 34.3% of sample F and 0.319, the therefore system of same blanc fixe dosage,
The covering power of sample E wants height.
For gloss:
Sample E and F be respectively 23.2% and 35.5% more than the percentage composition of 350nm granule number, therefore goods
Glossy specimen E is more than sample F.
The result of above-mentioned covering power and gloss and blanc fixe industry and the cognition of downstream application industry technology personnel
Result is completely the same, i.e. sample E (trade mark is Blanc Fixe Micro) is famous the going for industrial paint etc. in the whole world
Industry can substitute 7～the titanium dioxide of 10% and the most do not reduce the covering power of product and the product of gloss；Sample F (is produced
Ground is for Hunan) be the product of domestic good quality level, its in industrial paint to the substitution rate of titanium dioxide 3～5%.
Two samples of sample E and F are carried out application test detection and has verified particle diameter distribution and particle morphology statistics
The accuracy of result.Table 4 is applying detection result.
Table 4 applying detection result
In table 4, covering power and gloss in acrylic paint use following methods to detect:
In 200ml vial, add 100g bead, add the component in every formula in table 4, after sealing
On vibration mill, grinding distribution to scraper plate is read in detail and is reached 10 microns, makes paint.Then 5g paint is taken micro-with 60
The bar spreader of rice carries out film in black and white paperboard, for ensureing the accuracy of result, is coated with membrane process and uses automatically
Film applicator film.After natural drying 24 hours, measure the contrast ratio of film (paint film).The survey of paint film contrast ratio
It is fixed that according to GB/T 13452.3-1992, " the mensuration Part I of paint and varnish covering power is suitable to white and light color
The Kubelka-Munk method of paint " it is measured.
Result verification from Tables 1 and 2 goes out particle diameter between blanc fixe theory and or the particle diameter model of actual requirement
The highest then covering power of number of particles percentage ratio enclosing (200～350nm) is the highest, more than the percentage of 350nm granule number
The highest then glossiness of content is the poorest.
It is emphasized that volume mean diameter D [4,3] is to calculate according to the computational methods of laser particle analyzer in table 3
The particle diameter gone out, invents for edition with parallel text, does not the most substantially exist with downstream application effect and significantly associate
Property.
Claims (10)
1. the Particle Size Determination Method of the irregular powder body material of particle morphology, it is characterised in that: comprise the steps of,
A: joined by the powder body material insoluble in solvent and make the slurry that mass concentration is 20～70% in solvent, adds dispersant and abrasive media is ground dispersion and processes；
B: take slurry described in part steps A and add the suspension that solvent dilution becomes mass concentration to be 0.2～2.5%, disperse 1～15 minute with ultrasound wave；
C: take the hanging drop described in step B with micropipettor or capillary tube and be added to band and support that the transmission electron microscope special purpose copper of film is online, makes particle tile and dried on copper mesh uses TEM observe and make photo；
D: the maximum gauge of 1000～10000 particles in employing craft or software measurement photo and minimum diameter, the then distribution of statistics particle diameter and particle morphology；
In step A, oil absorption being less than to the powder body of 30g/100g, preferably grinding concentration is 40～65%, and dispersant dosage is the 1～5% of powder quality；For the oil absorption powder body more than 30g/100g, preferably grinding concentration is 30～50%, and dispersant dosage is the 2～10% of powder quality.
The Particle Size Determination Method of the irregular powder body material of particle morphology the most according to claim 1, it is characterised in that: in step A, the sampling amount of powder body material is not less than 2g.
The Particle Size Determination Method of the irregular powder body material of particle morphology the most according to claim 1, it is characterised in that: the solvent in step A and B is ethanol；One during dispersant is the NUOSPERSE FA196 of BYK111, Hai Mingsi company of Bi Ke company, polyvinylpyrrolidone in step A；Abrasive media is zirconium pearl.
4. according to the Particle Size Determination Method of the irregular powder body material of particle morphology described in claim 1 and 2, it is characterised in that: abrasive media is 0.8:1～3:1 with the mass ratio of slurry, and the diameter range of abrasive media is 0.4mm～2.0mm.
The Particle Size Determination Method of the irregular powder body material of particle morphology the most according to claim 1, it is characterized in that: in step A, grinding distribution processes is to carry out in sand mill or vibration mill, and the terminal that dispersion processes is that Hegman grind gage measures fineness less than 5 microns.
The Particle Size Determination Method of the irregular powder body material of particle morphology the most according to claim 1, it is characterised in that: for the powder body that particle diameter is 0.01～0.8 micron in step B, diluted concentration is 0.2～1.2%；It is 0.8～2.0% for the particle diameter powder body diluted concentration more than 0.8 micron.
Particle Size Determination Method the most according to claim 1, it is characterised in that: in step C, the volume of the suspension that micropipettor or capillary tube pipette is 0.5～50 microlitres, drips to tiling on copper mesh for disposable dropping 1～2 and be dried when being added drop-wise to copper mesh.
Particle Size Determination Method the most according to claim 1, it is characterised in that: the support film thickness that the TEM special purpose copper used in step C covers on the net is less than 20nm.
Particle Size Determination Method the most according to claim 1, it is characterised in that:
In step D, the maximum gauge of each particle in photo and the measuring method of minimum diameter are: find two points of furthest apart on particle shape projection line, A and B, and be linked to be a line segment AB；Drawing circle with AB for diameter, this circle, by tangent with A, the B 2 on particle shape projection line, checks whether A, B 2 is 2 farthest points, if it is, the distance of A, B 2 is maximum gauge；Drawing straight line, the midpoint of this straight-line pass AB is also perpendicular to AB, intersects at E and F with particle shape projection line, and the distance that E, F are 2 is minimum diameter.
Particle Size Determination Method the most according to claim 9, it is characterised in that: the particle diameter that in step D, the statistics of particle diameter distribution uses is maximum gauge；Particle morphology uses form factor F value to represent, each particle i.e. uses minimum diameter press the volume of spheroid calculating and the ratio of volume that maximum gauge is calculated by spheroid；The statistics of particle diameter distribution and particle morphology uses point three intervals to add up respectively, i.e. calculate the percentage composition shared by this number of particles after the number of particles in the particle size range of statistics coincidence theory and/or actual requirement, and calculate the arithmetic mean of instantaneous value of this scope particle F value；Statistics calculates the percentage composition shared by this number of particles after the number of particles less than theory and/or the particle size range of actual requirement, and calculates the arithmetic mean of instantaneous value of this scope particle F value；And calculate the percentage composition shared by this number of particles after the number of particles that statistics is more than theory and/or the particle size range of actual requirement, and calculate the arithmetic mean of instantaneous value of this scope particle F value.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410015067.2A CN103760074B (en) | 2014-01-13 | 2014-01-13 | The Particle Size Determination Method of the irregular powder body material of particle morphology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410015067.2A CN103760074B (en) | 2014-01-13 | 2014-01-13 | The Particle Size Determination Method of the irregular powder body material of particle morphology |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103760074A CN103760074A (en) | 2014-04-30 |
| CN103760074B true CN103760074B (en) | 2016-08-31 |
Family
ID=50527349
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410015067.2A Active CN103760074B (en) | 2014-01-13 | 2014-01-13 | The Particle Size Determination Method of the irregular powder body material of particle morphology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103760074B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109916930A (en) * | 2019-03-27 | 2019-06-21 | 龙蟒佰利联集团股份有限公司 | A method of test titanium dioxide internal layer silicon fiml pattern |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104198343A (en) * | 2014-09-12 | 2014-12-10 | 浙江浙能催化剂技术有限公司 | Detection method for particle size distribution of titanium dioxide |
| CN104390895B (en) * | 2014-11-25 | 2017-02-22 | 中国科学技术大学 | Microimaging-based method for measuring particle size by utilizing image gray scale |
| CN106501137B (en) * | 2015-09-07 | 2019-06-14 | 济南微纳颗粒仪器股份有限公司 | A kind of laser particle analyzer and method measuring particle sphericity |
| CN105445153B (en) * | 2015-12-24 | 2018-11-13 | 上海微谱化工技术服务有限公司 | The Particle size analysis methods of carbon black in PET |
| CN105865990B (en) * | 2016-03-28 | 2018-08-28 | 河南省人造金刚石微粉质量监督检验中心 | A kind of diadust grain size analysis sampling quantitative approach |
| CN105928849A (en) * | 2016-04-26 | 2016-09-07 | 长安大学 | Method for evaluating storage stability of penetrated oil layer emulsified asphalt |
| CN107576598B (en) * | 2017-09-15 | 2020-04-28 | 深圳市卡普瑞环境科技有限公司 | Method for acquiring quality of atmospheric particulate matter and terminal |
| CN109916941B (en) * | 2019-03-25 | 2021-04-30 | 苏州大学 | 3D printing separation detection method for premixed powder |
| CN110057650B (en) * | 2019-05-20 | 2022-03-15 | 常德力元新材料有限责任公司 | Method for evaluating steel strip crystal grains |
| CN110208151A (en) * | 2019-06-06 | 2019-09-06 | 中国科学院金属研究所 | The selective laser fusing detection method of titanium alloy ultra-fine Powder Particle Size and sphericity |
| CN110411920A (en) * | 2019-08-22 | 2019-11-05 | 攀钢集团攀枝花钢铁研究院有限公司 | The detection method of titanium white first product granularity |
| CN111474089A (en) * | 2020-04-23 | 2020-07-31 | 佛山市优一家电制造有限公司 | Water molecule particle size testing method and device of water vapor release equipment |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19948559C1 (en) * | 1999-10-08 | 2001-02-01 | Bat Cigarettenfab Gmbh | Particle detection method for tobacco particle stream e.g. in cigarette manufacturing machine, evaluates blocking of scanning beam by detected particles for calculating particle mean size and mean volume |
| CN101799393B (en) * | 2010-01-28 | 2012-11-21 | 天津大学 | Automatic quantitative evaluation method of microstructure character of particulate matters discharged by diesel engine |
| CN103196802B (en) * | 2013-03-27 | 2015-08-26 | 中国矿业大学(北京) | A kind of measuring method of filler sheet layer material radius-thickness ratio |
-
2014
- 2014-01-13 CN CN201410015067.2A patent/CN103760074B/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109916930A (en) * | 2019-03-27 | 2019-06-21 | 龙蟒佰利联集团股份有限公司 | A method of test titanium dioxide internal layer silicon fiml pattern |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103760074A (en) | 2014-04-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103760074B (en) | The Particle Size Determination Method of the irregular powder body material of particle morphology | |
| Heath et al. | Estimating average particle size by focused beam reflectance measurement (FBRM) | |
| CN101945824B (en) | Method of making zirconia-containing nanoparticles | |
| CN103965699B (en) | Adjustable without iris schemochrome pigment and preparation method thereof based on sepia | |
| CN105092571B (en) | A kind of quick determination method of oil paint system titanium dioxide application performance | |
| KR101706445B1 (en) | Process for preparing self-binding pigment particles | |
| CN102822664A (en) | Method of characterising scattering coloured pigment | |
| CN104428464B (en) | At rising temperature, there is high solid and the low viscosity aqueous slurry containing the calcium carbonate material that improve rheological stability | |
| CN107132162A (en) | A kind of particle diameter of alkaline earth metal carbonate powder and the assay method of particle diameter distribution | |
| CN109443864A (en) | The method for making sample of titanium dioxide weatherability detection | |
| CN109071963A (en) | The preparation of blooming and printing ink | |
| CN106226204A (en) | The detection method of metatitanic acid particle diameter | |
| Merkus et al. | Particle size, size distributions and shape | |
| Areias et al. | Polymer nanoparticle-based spherical photonic pigments for dye-free noniridescent bright coloring | |
| CN108956494A (en) | A kind of method of sulfate radical content in quick measurement bauxite | |
| CN107298876A (en) | A kind of preparation method of pearlescent pigment | |
| CN106970008A (en) | The method for determining ibuprofen pharmaceutical particle size and its distribution in ibuprofen suspension | |
| US6236460B1 (en) | Method to determine light scattering efficiency of pigments | |
| CN106018294B (en) | A method of detection nano-titanium dioxide down flop property | |
| CN104190313A (en) | A cost-reducing wetting dispersant used for titanium dioxide | |
| Juuti et al. | Light scattering study from nanoparticle-coated pigments of paper | |
| Liu et al. | Spectrometric characterization of suspension liquid and light extinction model update | |
| McGarvey et al. | Particle size analysis by laser diffraction in organic pigment technology | |
| CN110530517A (en) | It is a kind of using dimethyl silicone polymer as the natural minerals pigment color difference test method of substrate | |
| CN104764720B (en) | Method for comparing transparency of nanometer titanium dioxide and preparation method of composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 212009 Jiangsu province Zhenjiang new Dingmao Road No. 468 by twelve twin tower A Applicant after: INTER-CHINA CHEMICAL TECHNOLOGY CO., LTD. Address before: Zhenjiang City, Jiangsu province 212009 Dingmao Road No. 116 Building 1 Room 601 China Applicant before: INTER-CHINA CHEMICAL CO., LTD. |
|
| COR | Change of bibliographic data | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170210 Address after: 212009 Zhenjiang City, Jiangsu province Dingmao Jingkou District by fifteen Road No. 99 Building No. 19 Patentee after: Jiangsu new Mstar Technology Ltd Patentee after: Zhenjiang panchina Detection Technology Co. Ltd. Patentee after: INTER-CHINA CHEMICAL TECHNOLOGY CO., LTD. Address before: 212009 Jiangsu province Zhenjiang new Dingmao Road No. 468 by twelve twin tower A Patentee before: INTER-CHINA CHEMICAL TECHNOLOGY CO., LTD. |
|
| TR01 | Transfer of patent right |