CN105924175B - A kind of fine grain boron carbide ceramics and preparation method thereof - Google Patents

A kind of fine grain boron carbide ceramics and preparation method thereof Download PDF

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CN105924175B
CN105924175B CN201610250599.3A CN201610250599A CN105924175B CN 105924175 B CN105924175 B CN 105924175B CN 201610250599 A CN201610250599 A CN 201610250599A CN 105924175 B CN105924175 B CN 105924175B
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boron carbide
powder
carbide ceramics
fine grain
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CN105924175A (en
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张志晓
张晓荣
田仕
何强龙
王爱阳
王为民
傅正义
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Hebei University of Engineering
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    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/563—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on boron carbide
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Abstract

The present invention relates to a kind of fine grain boron carbide ceramics and preparation method thereof, belong to technical field of ceramic material.The fine grain boron carbide ceramics average grain size is less than 1 μm, and relative density, 98% or more, Vickers hardness is in 38GPa or more, and fracture toughness is in 4.9MPa.m1/2More than, preparation method is using boron powder and carbon dust as raw material, and idiosome is made in gained powder after mechanochemistry is handled, and the reaction raw materials of the green external package self- propagating system obtain fine grain boron carbide ceramics by self propagating high temperature Quick-pressing sintering technology.Boron carbide ceramics prepared by the present invention possesses that crystallite dimension is small, compactness is high, toughness is high, advantage with high hardness；The processing route simple process, yield is not high, time-consuming short, high to raw material particle size size requirements simultaneously, therefore cost is relatively low, is conducive to industrialized production.

Description

A kind of fine grain boron carbide ceramics and preparation method thereof
Technical field
The present invention relates to boron carbide ceramics material and preparation method thereof more particularly to a kind of fine grain boron carbide ceramics and its systems Preparation Method belongs to technical field of ceramic material.
Background technique
Boron carbide ceramics is a kind of important engineering material, in addition to Common advantages (wear-resistant, the anti-corruption with structural ceramics Erosion, high temperature resistant etc.) outside, advantage the most prominent is exactly to have the hardness and low density of superelevation simultaneously.At room temperature, it is carbonized The hardness of boron is only second to diamond and cubic boron nitride and occupies third, however, at high temperature (more than 1300 DEG C), boron carbide Hardness can be more than diamond and cubic boron nitride and become first.In addition, the density of boron carbide only has 2.52g/cm3, only steel 1/3 or so of iron is lower than most of ceramic materials.The ultrahigh hardness of boron carbide and it is Lightness make its modern industry, aviation navigate There is highly important application prospect in it and national defense construction field.However, since covalently linkage content is up in carbonization boron crystal 93.9%, and its plasticity is poor, crystal boundary moving resistance is big, surface tension very little when solid-state, therefore the fracture of boron carbide ceramics is tough Property it is lower, densification sintering temperature is excessively high, is difficult using pressureless sintering even if the high temperature more than 2200 DEG C to obtain consistency Boron carbide block more than 95%, this brings extreme difficulties for the preparation and application of boron carbide ceramics.
For ceramic material, fracture toughness is improved, the general technology means that lower sintering temperature is taken are refinements Material grains, addition sintering aid and second-phase dispersion reinforcement technique.However, for boron carbide ceramics, current research It mostly concentrates on through addition sintering aid or second-phase dispersion distribution technique is used to prepare boron carbide base composite ceramic to improve it Fracture toughness reduces sintering temperature.But in composite ceramics, since the hardness of the second phase is both less than boron carbide, density is both greater than Boron carbide, therefore the introducing of the second phase can reduce the hardness of boron carbide ceramics, while destroy the Lightness of boron carbide ceramics, because This, some excellent properties of boron carbide one-component ceramic can be sacrificed by preparing boron carbide composite ceramic.Although single-phase boron carbide ceramics material Material has its irreplaceable advantage, but refines boron carbide crystal grain mode at present to improve the research of its fracture toughness to use It is less, reason are as follows: 1, the acquisition of thin boron carbide powder it is very difficult, general industry production boron carbide powder partial size be greater than 3 μm, it is sintered using this powder, boron carbide ceramics of the size of microcrystal less than 3 μm can not be prepared；Although 2, using advanced Flouring technology can prepare the boron carbide powder of partial size smaller (less than 1 μm), but its cost is excessively high, yield and small, can only Use laboratory research；Even if 3, using small particle boron carbide powder for raw material, since pure boron carbide material sintering densification is difficult, Common sintering process (pressureless sintering, hot pressed sintering, discharge plasma sintering etc.) needs high sintering temperature, causes to be carbonized Boron crystal grain is grown up, and fine grain boron carbide ceramics can not be still obtained.Therefore, the report for preparing pure boron carbide ceramics is less.Though currently, So there is the relevant report for preparing pure boron carbide ceramics on a small quantity, but the Sinter of Boron Carbide Ceramics temperature prepared by it is higher, crystal grain It is larger, the pure boron carbide ceramics of fine grain can not be obtained, so that the fracture toughness of boron carbide ceramics can not be improved.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of fine crystalline carbon in view of the deficiency of the prior art Change boron ceramics and preparation method thereof, the preparation process is simple, and high-efficient and energy consumption is low, and prepared fine grain boron carbide ceramics are average Crystallite dimension possesses high rigidity and higher fracture toughness less than 1 μm.
The present invention be solve the problems, such as it is set forth above used by technical solution are as follows:
A kind of fine grain boron carbide ceramics, average grain size is less than 1 μm, and relative density is 98% or more, Vickers hardness For 38GPa or more, fracture toughness 4.9MPa.m1/2More than.
The preparation method of above-mentioned fine grain boron carbide ceramics is to handle using boron powder and carbon dust as raw material by mechanochemistry Idiosome is made in gained amorphous B-C nano-powder afterwards, and the reaction raw materials of the green external package self- propagating system pass through self- propagating High temperature Quick-pressing sintering technology obtains fine grain boron carbide ceramics.
Preferably, the preparation method of the fine grain boron carbide ceramics is using boron powder and carbon dust as raw material, by mechanization Idiosome is made in gained amorphous B-C nano-powder after processing, and the reaction raw materials of the green external package self- propagating system pass through Cause self-propagating reaction supply amorphous B-C nano-powder transformation and generate the nanocrystalline institute's calorific requirement of boron carbide, then by pressure, heat Processing is to obtain fine grain boron carbide ceramics.
Preferably, the preparation method of the fine grain boron carbide ceramics, includes the following steps:
1) by weight percentage, weighing boron powder 78-79%, carbon dust 21-22% is raw material, carries out mechanochemistry processing Afterwards, amorphous B-C nano-powder is obtained；
2) gained amorphous B-C nano-powder is pressed into interior embryo；
3) carbon dust 18%-20%, titanium valve 72%-80%, carbonized titanium powder 0-10% by weight percentage, are weighed, is mixed Uniformly, the material powder of self- propagating system is obtained；
4) material powder of self- propagating system obtained by step 3) will be superscribed outside embryo in step 2) gained and be pressed into multiple Embryo, then ignite self-propagating reaction, and (self-propagating reaction is combined with pressure, as from climing for pressure compacting immediately after reaction Prolong high temperature Quick-pressing sintering technology), it is released stress after temperature is lower than 1200 DEG C, obtains boron carbide block material after cooling Material；
5) boron carbide block materials obtained by step 4) are heat-treated, obtain fine grain boron carbide ceramics.
According to the above scheme, mechanochemical treatment step described in step 1) uses ball-milling technology.Specifically, ball-milling technology Are as follows: ball material mass ratio is 20:1-40:1, and rotational speed of ball-mill 300-500rpm, Ball-milling Time 30-50h, entire mechanical milling process is lazy It is carried out in property atmosphere.
According to the above scheme, washing and drying are include thed steps that between the step 1) and step 2).Preferably, described Washing includes pickling and washing；The drying is vacuum drying.Specifically, the pickling are as follows: the hydrochloric acid solution at 40 DEG C It is filtered after middle stirring；The washing is to dissolve, stir in deionized water, is then filtered.
According to the above scheme, interior embryo described in step 2) and multiple embryo are preferably cylindric, the volume relationship of the two are as follows: multiple embryo height It is 6-8 times of interior embryo height, 6-10 times of diameter.For example, interior embryo is the cylindrical body of diameter 1-2cm, height 0.5-1cm, multiple embryo To be highly 6cm, diameter 10cm, cylindrical body, interior embryo 1-4 can be uniformly placed in a multiple embryo at this time.
According to the above scheme, it suppresses described in step 2) and is preferably first suppressed using the axial compressive force of 15-30MPa, then use 150- 300MPa carries out isostatic cool pressing processing.
According to the above scheme, carbon dust described in step 3), the preferred 1:4 of titanium valve mass ratio.
According to the above scheme, in step 4), the material powder of self- propagating system obtained by idiosome and step 3) obtained by step 2) it Between have wall.Preferably, the wall is graphite paper and/or boron nitride.
According to the above scheme, press described in step 4) compacting pressure be 150-200MPa axial compressive force, until reaction System temperature releases stress after being lower than 1200 DEG C, and the dwell time is usually 40-60s.
According to the above scheme, in step 5), the heat treatment temperature is 1400-1600 DEG C, time 1-2h.
According to the above scheme, the partial size of boron powder is 1-75 μm in the step 1), and purity is greater than 98%, and the partial size of carbon dust is 0.1-3 μm, purity is greater than 99%.
Basic principle of the invention is as follows:
Firstly, raw material carbon dust and boron powder simple substance powder after mechanochemical process, can synthesize amorphous state, high activity B-C nano-powder.The nano-powder is in unstable noncrystalline state, and having sintering activity height, energy Spontaneous conversion is carbonization The trend of boron crystal.
Then, the present invention uses self propagating high temperature Quick-pressing sintering technology, carries out to amorphous B-C nano-powder idiosome fast Speed sintering, i.e., using carbon-titanium system as self-propagating combustion system, carbon-titanium system has reaction temperature height, and (maximum temperature is up to 3000 DEG C or more), the advantages of duration short (keeping 50s or so in 2200 DEG C of temperatures above) can, and can be by carbon-titanium system Titanium carbide powder is added with diluting reaction system, to achieve the purpose that regulate and control reaction temperature and reaction time.In addition, being somebody's turn to do from climing Reducing atmosphere can be generated by prolonging after combustion system ignites, under high temperature reducing atmospheres, it is ensured that boron carbide sample can be not oxidized. During self-propagating reaction, heating rate is up to 3000 DEG C/min or more, and amorphous B-C nano-powder is quick in temperature-rise period It is transformed into boron carbide nanocrystal, reaction moment completes.Under high temperature, just base is in red soft state to built-in boron carbide, at this point, The high pressure of one 150-200MPa of fast application, and continue 1 minute or so, make boron carbide sample densification, thus disposable complete Synthesis and densification process at boron carbide ceramics.Fast by heating rate, soaking time is short, during capable of effectively inhibiting sintering The boron carbide nanocrystal of the progress of flooding mechanism, formation has little time to grow up, and has just been pressed into ceramic block by high pressure, main Densification Mechanism is no longer mass transfer but red heat state sample generates Grain Boundary Sliding and plastic deformation under high pressure, thus The crystal grain of sample prepared by the technique will not obviously grow up during the sintering process, so that boron carbide be made to keep lesser crystal grain ruler It is very little.
After the sintering of self propagating high temperature Quick-pressing, although boron carbide ceramics is densified, since it is by non-crystalline flour Body fast transition, the temperature-rise period being exceedingly fast and extremely short sintering process cause the crystallinity of its crystal not so good, influence Its mechanical performance, therefore, it is necessary to carry out subsequent heat treatment to it, treatment temperature is at 1400-1600 DEG C, the heat of this range Reason temperature can make its crystal structure degree perfect, but not its crystal grain is caused to be grown up, and therefore, boron carbide ceramics obtained has Thin crystallite dimension and good crystallinity, and aplitic texture is conducive to improve the fracture toughness and hardness of boron carbide.
Compared with prior art, beneficial effects of the present invention are as follows:
First, the present invention can prepare the pure boron carbide ceramics with fine grain without thin boron carbide powder, should Ceramic crystalline grain size is less than 1 μm, and compactness is high, hardness is high, fracture toughness is preferable.
Second, the present invention prepares amorphous B-C nano-powder using mechanochemical reaction, to guarantee quickly to add in self propagating high temperature It presses and realizes that the synthesis of nano boron carbide crystal grain, a closely knit step are completed in sintering process, compared with conventional sintering means, possess heating Speed is fast, and sintering time is short, and consume energy low advantage.
Third, material powder B powder of the invention and C need to pass through mechanochemical process, therefore want to the original size of raw material It asks lower, production cost can be reduced, and have no special requirements to the purity and partial size of self- propagating system powder, therefore production can be reduced Cost.
4th, present invention process is simple, and high-efficient, short preparation period is advantageously implemented industrial mass production.
Detailed description of the invention
Fig. 1 is the XRD diagram of 1 gained amorphous B-C nano-powder of the embodiment of the present invention and boron carbide, wherein (a) is mechanization It learns technique and obtains amorphous B-C nano-powder；(b) the boron carbide block materials that the sintering of self propagating high temperature Quick-pressing obtains； (c) The fine grain boron carbide ceramics obtained after Overheating Treatment.
Fig. 2 is 2 gained fine grain boron carbide ceramics section SEM of embodiment of the present invention figure.
Fig. 3 is the polishing of 2 gained fine grain boron carbide ceramics of the embodiment of the present invention, etched surface SEM figure.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention Content is not limited solely to the following examples.
Embodiment 1
A kind of preparation method of fine grain boron carbide ceramics, it the following steps are included:
1) the B-C nano-powder of amorphous disordered structure is prepared
By weight percentage, 78% boron powder (partial size is 75 μm, purity 99%) and 22% carbon dust (partial size will be weighed It is 3 μm, purity 99%) it is put into progress mechanochemistry processing in the ball grinder of planetary ball mill, ball grinder is vacuumized After be filled with argon gas processing, ball grinder and ball material are stainless steel, and ball, material mass ratio are 30:1, and rotational speed of ball-mill is 500 rpm, ball Time consuming is 30h, obtains amorphous B-C nano-powder；
The amorphous B-C nano-powder that will acquire stirs 6h in the hydrochloric acid solution of 2mol/L at 40 DEG C, is then taken out Filter after dissolving, filtering in deionized water again by the powder filtered out, is placed in 60 DEG C of vacuum ovens for 24 hours to get to purifying Amorphous B-C nano-powder；
2) embryo in preparing
Amorphous B-C nano-powder is pressed into the disk of diameter 1cm, height 0.5cm under the axial compressive force of 20MPa, so Disk is put into cold equal press afterwards and carries out 200MPa, the isostatic cool pressing processing of 5min obtains the nanocrystalline interior embryo of amorphous B-C；
3) self- propagating system material powder is prepared
By weight percentage, carbon dust 18%, titanium valve 72%, carbonized titanium powder 10% are weighed, is obtained after mixing from climing Prolong system material powder；
4) self propagating high temperature Quick-pressing is sintered
The interior embryo outer layer that step 2) obtains successively is superscribed into graphite paper and boron nitride powder, it is then that 4 interior embryos are uniform Be placed in the resulting self- propagating system material powder of step 3), be pressed into height be 6cm, the multiple embryo that diameter is 10cm, by institute It states multiple idiosome to be placed in self propagating high temperature Quick-pressing equipment, ignite self-propagating reaction, and applies the axis of 150MPa in 60s To pressure, temperature is lower than 1200 DEG C after pressure maintaining 40s, releases stress rear natural cooling, obtains boron carbide block materials；
5) boron carbide block is heat-treated
The boron carbide block materials that step 4) obtains are put into the high temperature furnace of argon atmosphere and are heat-treated, heat treatment temperature Degree is 1400 DEG C, time 2h, obtains fine grain boron carbide ceramics.
The performance of fine grain boron carbide ceramics sample obtained by the present embodiment is as follows: relative density 99.1%, Vickers hardness 38.1GPa, fracture toughness 4.96MPa.m1/2, 0.89 μm of average grain size.
Embodiment 2
A kind of preparation method of fine grain boron carbide ceramics, it the following steps are included:
1) the B-C nano-powder of amorphous disordered structure is prepared
By weight percentage, 79% boron powder (partial size is 1 μm, purity 98%) and 21% carbon dust (partial size will be weighed It is 0.1 μm, purity 99%) it is put into progress mechanochemistry processing in the ball grinder of planetary ball mill, ball grinder take out true Argon gas processing is filled with after sky, ball grinder and ball material are stainless steel, and ball, material mass ratio are 30:1, and rotational speed of ball-mill is 400 rpm, Ball-milling Time is 50h, obtains amorphous B-C nano-powder；
The amorphous B-C nano-powder that will acquire stirs 6h in the hydrochloric acid solution of 2mol/L at 40 DEG C, is then taken out Filter after dissolving, filtering in deionized water again by the powder filtered out, is placed in 60 DEG C of vacuum ovens for 24 hours to get to purifying Amorphous B-C nano-powder；
2) embryo in preparing
Amorphous B-C nano-powder is pressed into the disk of diameter 2cm, height 1cm under the axial compressive force of 20MPa, then Disk is put into cold equal press and carries out 200MPa, the isostatic cool pressing processing of 5min obtains the nanocrystalline interior embryo of amorphous B-C；
3) self- propagating system material powder is prepared
By weight percentage, carbon dust 20%, titanium valve 80% are weighed, obtains self- propagating system raw material powder after mixing Body；
4) self propagating high temperature Quick-pressing is sintered
The interior embryo outer layer that step 2) obtains successively is superscribed into graphite paper and boron nitride powder, it is then that 1 interior embryo is uniform Be placed in the resulting self- propagating system material powder of step 3), be pressed into height be 6cm, the multiple embryo that diameter is 10cm, by institute It states multiple idiosome to be placed in self propagating high temperature Quick-pressing equipment, ignite self-propagating reaction, and applies the axis of 200MPa in 40s To pressure, pressure maintaining 60s temperature is lower than 1200 DEG C, releases stress rear natural cooling, obtain boron carbide block materials；
5) boron carbide block is heat-treated
The boron carbide block materials that step 4) obtains are put into the high temperature furnace of argon atmosphere and are heat-treated, heat treatment temperature Degree is 1600 DEG C, time 1h, obtains fine grain boron carbide ceramics.
The performance of fine grain boron carbide ceramics sample obtained by the present embodiment is as follows: relative density 99.6%, Vickers hardness 39.8GPa, fracture toughness 4.92MPa.m1/2, 0.87 μm of average grain size.
Embodiment 3
The present embodiment and embodiment 2 the difference is that: in step 3), carbon dust 19%, titanium valve 76%, carbonized titanium powder 5%.
Embodiment 4
The present embodiment and embodiment 2 the difference is that: in step 3), carbon dust 18%, titanium valve 72%, carbonized titanium powder 10%.
The relative density, Vickers hardness of fine grain boron carbide ceramics prepared by 2-4 of the embodiment of the present invention, fracture toughness and crystalline substance Particle size is as shown in table 1:
1 fine grain boron carbide ceramics properties of table
The characteristics of fine grain boron carbide ceramic material prepared by the present invention is specifically introduced below with reference to legend (including it is relatively close Degree, Vickers hardness, fracture toughness and average grain size).
The present invention prepares amorphous by mechanochemical process using boron powder and carbon dust as raw material it can be seen from Fig. 1 (a) The XRD spectra of B-C nano-powder is a smooth curve, is illustrated after ball milling, material powder forms unformed Amorphous powder, and in this powder and do not include crystalline silicon carbide boron object phase.Within the scope of 15-25 °, 30-40 °, diffraction spectrogram goes out An existing more gentle peak packet, and this range is corresponding with the mutually main characteristic peak of boron carbide object, illustrates although powder does not have Carbonization boron crystal is formed, but forms distortion B-C key, is transitional face of the mixed powder to carbonization boron crystal.And from Fig. 1 (b) As can be seen that contain only the characteristic peak of boron carbide object phase in spectrogram, illustrate amorphous powder after self- propagating high-pressure sinter, shape At pure boron carbide object phase.However, the diffraction maximum that Fig. 1 (b) shows is weaker compared with Fig. 1 (c), illustrate only through self- propagating high pressure After sintering, the crystallinity of boron carbide sample is poor, and can significantly improve its crystal structure by subsequent heat treatment technique.
As seen from Figure 2, minimal amount of size is contained only in fine grain boron carbide ceramics sample prepared by the present invention to be less than The Minute pores of 100nm, sample are almost completely fine and close.
The crystallite dimension minimum that Fig. 3 can be seen that fine grain boron carbide ceramic material sample prepared by the present invention only has 0.3 μm Left and right, largest grain size are also no more than 1.5 μm, and average particle diameter size only has 0.87 μm, realizes the target of fine grain.
As can be seen from Table 1, the boron carbide ceramics that the present invention prepares has high solidity (> 98%), and high Vickers is hard It spends (> 38GPa), higher fracture toughness (> 4.9MPa.m1/2) and small crystallite dimension (average grain size < 1 μm), explanation The present invention has biggish advantage to preparation fine grain boron carbide ceramics；In addition, it could be seen that with diluent carbon in self- propagating system Change the increase of Ti content, ceramic relative density and Vickers hardness reduce, and fracture toughness increases, and average grain size without Significant change rule.This is because titanium carbide is a kind of diluent in self- propagating system, the increase of diluent can reduce reaction The reaction temperature of system and duration can adjust the partial properties of target sample by changing the content of diluent, still, The content of titanium carbide should not be too high, no more than 10%.
The above is only a preferred embodiment of the present invention, cited each raw material can realize the present invention, each raw material Bound value and its interval value can realize the present invention, present invention process parameter (such as proportion, temperature, time) it is upper Lower limit value and its interval value can realize the present invention, embodiment numerous to list herein.It should be pointed out that for this field For those of ordinary skill, without departing from the concept of the premise of the invention, several modifications and variations can also be made, these Belong to protection scope of the present invention.

Claims (6)

1. a kind of preparation method of fine grain boron carbide ceramics, it is characterised in that include the following steps:
1) by weight percentage, weighing boron powder 78-79%, carbon dust 21-22% is raw material, after carrying out mechanochemistry processing, is obtained Amorphous B-C nano-powder；Wherein, the mechanochemical treatment step uses ball-milling technology, ball-milling technology are as follows: ball material mass ratio is 20:1-40:1, rotational speed of ball-mill 300-500rpm, Ball-milling Time 30-50h, entire mechanical milling process carry out in an inert atmosphere；
2) gained amorphous B-C nano-powder is pressed into interior base；
3) carbon dust 18%-20%, titanium valve 72%-80%, carbonized titanium powder 0-10% by weight percentage, are weighed, is uniformly mixed, obtains The material powder of self- propagating system；
4) material powder of self- propagating system obtained by step 3) will be superscribed outside base in step 2 gained and be pressed into multiple base, so After ignite self-propagating reaction, pressure compacting immediately after reaction releases stress after temperature of reaction system is lower than 1200 DEG C, Boron carbide block materials are obtained after cooling；
5) boron carbide block materials obtained by step 4) are heat-treated, obtain fine grain boron carbide ceramics.
2. a kind of preparation method of fine grain boron carbide ceramics according to claim 1, it is characterised in that described in step 2 Compacting is first suppressed using the axial compressive force of 15-30MPa, then carries out isostatic cool pressing processing using 150-300MPa.
3. a kind of preparation method of fine grain boron carbide ceramics according to claim 1, it is characterised in that in step 4), step 2) have a wall between the material powder of self- propagating system obtained by gained green body and step 3), the wall be graphite paper and/ Or boron nitride.
4. a kind of preparation method of fine grain boron carbide ceramics according to claim 1, it is characterised in that the interior base and multiple Base is cylindric, the volume relationship of the two are as follows: multiple base height is 6-8 times, 6-10 times of diameter of interior base height.
5. a kind of preparation method of fine grain boron carbide ceramics according to claim 1, it is characterised in that in step 4), pressure The pressure of compacting is the axial compressive force of 150-200MPa；In step 5), the heat treatment temperature is 1400-1600 DEG C, and the time is 1-2 h。
6. a kind of preparation method of fine grain boron carbide ceramics according to claim 1, it is characterised in that in the step 1) The partial size of boron powder is 1-75 μm, and purity is greater than 98%, and the partial size of carbon dust is 0.1-3 μm, and purity is greater than 99%.
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