CN106117229B - A kind of preparation method of speciality Hexanitrohexaazaisowurtzitane - Google Patents
A kind of preparation method of speciality Hexanitrohexaazaisowurtzitane Download PDFInfo
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- CN106117229B CN106117229B CN201610797488.4A CN201610797488A CN106117229B CN 106117229 B CN106117229 B CN 106117229B CN 201610797488 A CN201610797488 A CN 201610797488A CN 106117229 B CN106117229 B CN 106117229B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains four or more hetero rings
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Abstract
The invention provides a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane, comprise the following steps：Hexanitrohexaazaisowurtzitane material solution is provided；Stirred after the Hexanitrohexaazaisowurtzitane material solution stream is added into diluent, obtain speciality Hexanitrohexaazaisowurtzitane；The particle diameter of the speciality Hexanitrohexaazaisowurtzitane is 100~110 μm；The speed of the stirring is 500~600rpm；The diluent is low-carbon alkanes.Method provided by the invention improves the activity of the solutes of CL 20 in the solution, promotes the dissolving of metastable crystal formation, is advantageous to the growth of stable crystal form, and is advantageous to reduce the difference of growth rate between each crystal in crystallization process, and then improves the uniformity of grain size；Add order and mixing speed to prepare speciality CL 20 with the stream limited, change the natural habit of crystal, enable the synchronous growth as far as possible of each crystal face, so as to obtain spherical crystal particle.
Description
Technical field
The present invention relates to explosive field, more particularly to a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane.
Background technology
Hexanitrohexaazaisowurtzitane, be by Nielen of USN's weapons center et al. by for many years make great efforts in
Take the lead in synthesizing within 1987, be the Typical Representative of high-energy-density energetic material.
Hexanitrohexaazaisowurtzitane (CL-20) is polymorph, have four kinds of crystal formations for α, β, γ under normal temperature and pressure and
The crystalline density of ε, ε type Hexanitrohexaazaisowurtzitane reaches 2.04g/cm3~2.05g/cm3, there is excellent energy response,
Because its chemical stability is good, paid attention in again by domestic and international energetic material field, available for missile armament powder charge, solid
The field containing energy such as propellant and atom bomb priming.
The CL-20 that existing process produces to obtain is mostly ε crystal formations, and its crystal shape is mostly elongated bipyramid shape, median
About 40 microns, particle diameter distribution is wide, uneven.For example, often method synthesizes Hexanitrohexaazaisowurtzitane to existing process in two steps：
Six substitution hexaazaisopen wootz alkyls are synthesized by original amine first, then directly nitrified by six substitution hexaazaisopen wootz alkyls
Reaction production Hexanitrohexaazaisowurtzitane, obtains the Hexanitrohexaazaisowurtzitane of ε crystal formations, and particle diameter distribution is uneven,
Poor controllability.But in actual applications, high-energy-density powder charge require crystal shape rule, 100 μm~110 μm of average grain diameter with
And the uniform CL-20 of particle diameter distribution.
The content of the invention
It is an object of the invention to provide a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane,
Preparation method provided by the invention obtain grain size be 100~110 μm the azepine of speciality hexanitro six different 5 hereby
Alkane, narrow particle size distribution, crystal shape rule are round and smooth.
The invention provides a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane, comprise the following steps：
Hexanitrohexaazaisowurtzitane material solution is provided；
Stirred after the Hexanitrohexaazaisowurtzitane material solution stream is added into diluent, obtain speciality hexanitro six
The hereby alkane of azepine different 5；The particle diameter of the speciality Hexanitrohexaazaisowurtzitane is 100~110 μm；The speed of the stirring is
500~600rpm；The diluent is low-carbon alkanes.
Preferably, the solvent in the Hexanitrohexaazaisowurtzitane material solution is monobasic acid ester.
Preferably, the mass ratio of the solute in the Hexanitrohexaazaisowurtzitane material solution and solvent is 1：(2.5
~3.5).
Preferably, the mass ratio of the diluent and solvent in the Hexanitrohexaazaisowurtzitane material solution is
(1.5~1.8)：1.
Preferably, the speed that the stream adds is (1.0~1.5) kg/min, and the temperature that the stream adds is 38~45 DEG C.
Preferably, the temperature of the stirring is 38~45 DEG C.
Preferably, the stream adds and the total time of the stirring is 2~3 hours.
Preferably, also include after the stirring：Diluent is added again into the feed liquid after the stirring.
Preferably, the diluent added again and solvent in the Hexanitrohexaazaisowurtzitane material solution
Mass ratio is (0.1~1):1.
Preferably, the temperature of the diluent is 38~45 DEG C.
The invention provides a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane, comprise the following steps：There is provided
Hexanitrohexaazaisowurtzitane material solution；After the Hexanitrohexaazaisowurtzitane material solution stream is added into diluent
Stirring, obtains speciality Hexanitrohexaazaisowurtzitane；The particle diameter of the speciality Hexanitrohexaazaisowurtzitane be 100~
110μm；The speed of the stirring is 500~600rpm；The diluent is low-carbon alkanes.Method provided by the invention is by CL-
20 solution streams are added to the restriction for the mixing speed that 500~600rpm is combined in low-carbon alkanes diluent, improve CL-20 solutes molten
Activity in liquid, promote the dissolving of metastable crystal formation, so as to be advantageous to the growth of stable crystal form, and be advantageous to reduction and crystallized
In journey between each crystal growth rate difference, and then improve grain size uniformity；The present invention is added suitable with the stream limited
Sequence and mixing speed prepare speciality CL-20, change the natural habit of crystal, each crystal face is synchronously given birth to as far as possible
It is long, so as to obtain spherical crystal particle.The embodiment of the present application result shows that resulting Hexanitrohexaazaisowurtzitane is brilliant
Volumetric laser narrow particle size distribution, grain shape rule, to be spherical, axial ratio is below 1.5, and circularity is more than 0.85, average grain
Footpath is 100~110 μm, meets high-energy-density powder charge requirement.
Further, the temperature control of the temperature of stream plus process, the temperature in whipping process and diluent, influences solution
The crystalline rate and growth rate of middle crystal, and then the stability of crystal is influenceed, within the temperature range of limiting, β-ε turn crystalline substance
Time is shorter, while avoids ε and turn crystalline substance to γ, overcomes energy required when resistance and supply cenotype generate in solid liquid interface
Amount, be advantageous to the diffusion of solute and solvent molecule in solvent, improve crystallization rate, promote crystal respectively to increase to uniform, avoid
Stable crystal form caused by temperature is too high is changed into metastable crystal formation.
Further, controlling stream adds the time of process and whipping process, it is ensured that crystal fully separates out, turns brilliant completion, control
The long time is made so that different crystal synchronous growth, and then obtain the crystal grain of even size distribution.
Further, the residual quantity that diluent reduces solute in CL-20 solution is added in the feed liquid after stirring again, is improved
Yield, and be added to using diluent in the feed liquid after stirring, degree of supersaturation increase is more gentle, separates out crystal mostly with original
It is crystal seed to have crystal, promotees its growth, is further ensured that the uniformity of crystal size distribution.
Brief description of the drawings
Fig. 1 is the micro-structure diagram of CL-20 in the prior art；
Fig. 2 is the micro-structure diagram for the speciality CL-20 that the embodiment of the present invention 1 obtains；
Fig. 3 is the laser particle size normal distribution of CL-20 preparing raw materials；
Fig. 4 is the Laser particle-size distribution figure for the special CL-20 that the embodiment of the present invention 1 obtains.
Embodiment
The invention provides a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane, comprise the following steps：There is provided
Hexanitrohexaazaisowurtzitane material solution；After the Hexanitrohexaazaisowurtzitane material solution stream is added into diluent
Stirring, obtains speciality Hexanitrohexaazaisowurtzitane；The particle diameter of the speciality Hexanitrohexaazaisowurtzitane be 100~
110μm；The speed of the stirring is 500~600rpm；The diluent is low-carbon alkanes.
Method provided by the invention, CL-20 solution streams are added to stirring with reference to 500~600rpm in low-carbon alkanes diluent
The restriction of speed is mixed, the activity of CL-20 solutes in the solution is improved, promotes the dissolving of metastable crystal formation, so as to be advantageous to stabilization
The growth of crystal formation, and be advantageous to reduce the difference of growth rate between each crystal in crystallization process, and then improve grain size
Uniformity；The present invention adds order and mixing speed to prepare speciality CL-20 with the stream limited, changes the natural growth of crystal
Habit, enable the synchronous growth as far as possible of each crystal face, so as to obtain spherical crystal particle.
Hexanitrohexaazaisowurtzitane material solution stream is added in diluent by the present invention.In the present invention, described six
Solvent in nitro hexaazaisopen wootz alkyl material solution is preferably monobasic acid ester, more preferably acetic acid esters, most preferably acetic acid
One or more in ethyl ester, methyl acetate and butyl acetate.In the present invention, the Hexanitrohexaazaisowurtzitane raw material
The mass ratio of solute and solvent is preferably 1 in solution：(2.5~3.5), more preferably 1：(3.1~3.4)；In the reality of the present invention
Apply in example, the mass ratio of solute and solvent can be specially 1 in the Hexanitrohexaazaisowurtzitane material solution:3.2、1:
3.3 or 1:3.4.The present invention does not have special want to the source of the solute in the Hexanitrohexaazaisowurtzitane material solution
Ask, using CL-20 preparing raw materials well-known to those skilled in the art.In the present invention, the raw material is elongated double ribs
Taper, circularities are less than 0.8, and particle diameter distribution is wide, and axial ratio is more than 1.5, and median is less than 50 μm.
The Hexanitrohexaazaisowurtzitane is preferably dissolved in the solvent by the present invention, in the present invention, described
The temperature of dissolving is preferably 20~30 DEG C, more preferably 21~24 DEG C.In the present invention, the dissolving is preferably in stirring bar
Carried out under part, the speed of the stirring is preferably 300~400rpm.
In the present invention, the course of dissolution is carried out preferably in dissolvers, in an embodiment of the present invention, the dissolving
Process is specifically carried out in dissolution kettle.
After the present invention preferably dissolves Hexanitrohexaazaisowurtzitane, obtained solution is filtered, removed wherein not
Molten impurity, obtain Hexanitrohexaazaisowurtzitane material solution.Present invention preferably employs the filter cloth of 500 mesh to the solution
Filtered.
The obtained solution is preferably transferred in head tank by the present invention, is realized by the control valve in the head tank
Add the control of process speed to rear afterflow.
In the present invention, the diluent is low-carbon alkanes, and preferably carbon number is 6~8 alkane, more preferably just
One or more in octane, normal heptane and n-hexane.In the present invention, the temperature of the diluent is preferably 38~45 DEG C,
More preferably 40~42 DEG C.The present invention is preferably by the way that diluent raw material is obtained in 25~35min of the temperature inside holding
Required diluent.In the present invention, the matter of the diluent and solvent in the Hexanitrohexaazaisowurtzitane material solution
Amount is than being preferably (1.5~1.8)：1, more preferably (1.6~1.7)：1.
After obtaining the diluent of the temperature, the Hexanitrohexaazaisowurtzitane material solution stream is added to by the present invention
Diluent.In the present invention, the speed that the stream adds is preferably (1.0~1.5) kg/min, more preferably (1.2~1.4)
kg/min.In the present invention, the temperature of the stream plus process is preferably 38~45 DEG C, more preferably 43~44 DEG C.At this
In invention, the temperature is preferably kept by the temperature of the solution flowed during adding and diluent, when the stream plus process
In solution and the temperature of diluent when being difficult to ensure that the temperature of the stream plus process, it is preferably real by way of the external world is heated
It is existing.
In the present invention, the stream plus process are carried out preferably in crystallization kettle, and the diluent specifically is placed in into crystallization
In kettle, stream plus Hexanitrohexaazaisowurtzitane material solution into the crystallization kettle.
After the present invention completion stream adds, it is stirred, obtains speciality CL-20 crystal.In the present invention, the stirring
Speed is 500~600rpm, more preferably 520~580rpm, most preferably 550~560rpm.In the present invention, it is described
The time of stirring is preferably 60~120min, more preferably 65~70min.In the present invention, the temperature of the stirring is excellent
Elect 38~45 DEG C, more preferably 40~44 DEG C as.The present invention does not have particular/special requirement to the concrete operation step of the stirring,
Using the technical scheme of stirring well-known to those skilled in the art.In the present invention, the stream plus process are in stirring bar
Carried out under part, improve dilution effect of the diluent to CL-20 solution.
In the present invention, the total time of the whipping process after the stream plus process and the stream add is preferably 2~3 hours,
Most preferably 2.5 hours.
After completing the stirring, the present invention preferably adds diluent again into the feed liquid after the stirring.In the present invention
In, the diluent and the mass ratio of solvent in the Hexanitrohexaazaisowurtzitane material solution that add again are preferably (0.1
~1):1, more preferably (0.5~0.7)：1.In the present invention, the temperature and species of the diluent added again
It is defined according to the above-mentioned diluent referred to.In the present invention, the diluent added again can reduce CL-20 solution
The residual quantity of middle solute, improve yield
After the secondary addition for completing the diluent, the present invention is preferred to carry out secondary agitation, completes crystallization.In the present invention
In, the speed of the secondary agitation is preferably 700~800rpm, more preferably 720~750rpm.In the present invention, institute
The temperature for stating secondary agitation process is preferably not lower than 38 DEG C, preferably 39~40 DEG C.
After completing the crystallization, the material after crystallization is preferably carried out separation of solid and liquid and drying by the present invention, obtains speciality CL-
20.The present invention does not have special limitation to the method for the separation of solid and liquid, the separation of solid and liquid that who knows using those skilled in the art
Technical scheme, such as can using filtering by the way of, more specifically can be filter.
In the present invention, the liquid phase part obtained after separation of solid and liquid preferably includes the solvent in diluent and CL-20 solution
Mixed solution.In the present invention, the concentration of diluent is preferably 30~50% in the liquid phase part, and more preferably 40
~45%.In the present invention, when the concentration of the liquid phase part is in the scope, ratio defective product is optimal.
In the present invention, the temperature of the drying is preferably 50 DEG C~55 DEG C, more preferably 52~53 DEG C；In this hair
In bright, the time of the drying is preferably 5~10 hours, more preferably 6~8 hours.In the present invention, the speciality
BTF moisture is preferably shorter than 0.10%.The embodiment of the present invention is specifically used and is dried in drying cupboard.
In order to further illustrate the present invention, with reference to embodiment to Hexanitrohexaazaisowurtzitane provided by the invention
Preparation method be described in detail, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
By taking 50 liters of glass crystallization kettles as an example, the CL-20 is using made of following steps：
1st, at room temperature, 10kg ethyl acetate is added in dissolution kettle；
2nd, under the stirring condition of 300rpm rotating speeds, 4 ㎏ CL-20 are added, observation CL-20 all dissolves；
3rd, lysate is filtered, lysate is added in head tank,
3rd, 16kg normal octanes are added in crystallization kettle, are warming up to 42 DEG C~45 DEG C；
4th, under 500rpm rotating speeds, CL-20 solution is added with 1.0kg/min speed, continues to stir 110min, control crystallization
Temperature is not less than 38 DEG C；
5th, blowing, the solvent in filtering layer is drained；
6th, crystallized stock is placed in drying cupboard drying, under conditions of 50 DEG C, is dried to moisture less than 0.10%；
7th, dry after material moisture it is qualified after, mix batch vanning；
8th, analytical control indices, after meeting the requirement of speciality CL-20 contract standards, packaging.
Obtained speciality CL-20 is carried out microstructure detection by the present invention, as a result as shown in Fig. 2 Fig. 2 is implemented for the present invention
The microstructure picture for the speciality CL-20 that example 1 obtains, by compared with prior art CL-20 microstructure (Fig. 1),
Crystal shape is mostly elongated bipyramid shape in Fig. 1, and particle diameter distribution is wide, about 40 microns of median；In Fig. 2, crystal to be spherical,
Surface is round and smooth, and without obvious corner angle, axial ratio is small, and no more than 1.5, circularities are high, and more than 0.85, granularity is big, average grain diameter
For 100~110 μm.
Size distribution detection is carried out to obtained speciality CL-20 by laser particle size analyzer, it is as a result as shown in figure 3, logical
Cross compared with raw material CL-20 size distribution in preparation process, it is known that, the speciality CL-20's obtained according to this programme swashs
D90=150 μm in light bead degree normal distribution, D10=60 μm, and D90=300 μm of CL20 raw material laser particle sizes normal distribution, D10
=20 μm, it is clear that the product Laser particle-size distribution that this programme obtains is narrower.
Analytical control indices, after meeting the requirement of speciality CL-20 contract standards, packaging, the indices such as embodiment of table 1
Shown in 1 obtained speciality CL-20 all technicals.
The all technical for the speciality CL-20 that the embodiment of the present invention 1 of table 1 obtains
| Sequence number | Index name | Index |
| 1 | Chemical purity (m/m) % >= | 99.00 |
| 2 | ε crystal form purities (m/m) % >= | 95.00 |
| 3 | Ethyl acetate insoluble matter (m/m) %≤ | 0.03 |
| 4 | Inorganic insoluble substance (m/m) %≤ | 0.02 |
| 5 | Acidity (in terms of nitric acid) (m/m) %≤ | 0.02 |
| 6 | Moisture and volatile matter (m/m) %≤ | 0.10 |
| 7 | D50 μm of laser particle size | 100~110 |
Embodiment 2
By taking 50 liters of glass crystallization kettles as an example, the CL-20 is using made of following steps：
1st, at room temperature, 10kg ethyl acetate is added in dissolution kettle；
2nd, under the stirring condition of 300rpm rotating speeds, 4 ㎏ CL-20 are added, observation CL-20 all dissolves；
3rd, lysate is filtered, lysate is added in head tank,
3rd, 16kg normal octanes are added in crystallization kettle, are warming up to 38 DEG C；
4th, under 500rpm rotating speeds, CL-20 solution is added with 1.0kg/min speed, continues to stir 1h；Again with 1.kg/min
Speed add 3.5kg normal octanes, with 700rpm rotating speed continue stir 1h, control crystallization temperature be not less than 38 DEG C；
5th, blowing, the solvent in filtering layer is drained；
6th, crystallized stock is placed in drying cupboard drying, under conditions of 50 DEG C, is dried to moisture less than 0.10%；
7th, dry after material moisture it is qualified after, mix batch vanning；
8th, analytical control indices, after meeting the requirement of speciality CL-20 contract standards, packaging.
Embodiment 3
By taking 50 liters of glass crystallization kettles as an example, the CL-20 is using made of following steps：
1st, under the conditions of 20 DEG C, 10kg ethyl acetate is added in dissolution kettle；
2nd, under the stirring condition of 300rpm rotating speeds, 3.5 ㎏ CL-20 are added, observation CL-20 all dissolves；
3rd, lysate is filtered, lysate is added in head tank,
3rd, 18kg normal octanes are added in crystallization kettle, are warming up to 45 DEG C；
4th, under 600r/min rotating speeds, CL-20 solution is added with 1.5kg/min speed, continues to stir 1h；Again with 1.5kg/
Min speed adds 3.5kg normal octanes, and 1h is stirred with 800rpm rotating speed, and it is 45 DEG C to control crystallization temperature；
5th, blowing, the solvent in filtering layer is drained；
6th, crystallized stock is placed in drying cupboard drying, under the conditions of 55 DEG C, is dried to moisture less than 0.10%；7th, after drying
Material moisture it is qualified after, mix batch vanning；
8th, analytical control indices, after meeting the requirement of speciality CL-20 contract standards, packaging.
Embodiment 4
By taking 50 liters of glass crystallization kettles as an example, the CL-20 is using made of following steps：
1st, under the conditions of 25 DEG C, 10kg ethyl acetate is added in dissolution kettle；
2nd, under the stirring condition of 300rpm rotating speeds, 3.3 ㎏ CL-20 are added, observation CL-20 all dissolves；
3rd, lysate is filtered, lysate is added in head tank,
3rd, according to solvent 1.7 in diluent and Hexanitrohexaazaisowurtzitane material solution：1 mass ratio is in crystallization kettle
Middle addition 17kg normal octanes, are warming up to 45 DEG C；
4th, under 600r/min rotating speeds, CL-20 solution is added with 1.0kg/min speed, continues to stir 1h；Again with 1.5kg/
Min speed adds 3.5kg normal octanes, and 1h is stirred with 800rpm rotating speed, and it is 42 DEG C to control crystallization temperature；
5th, blowing, the solvent in filtering layer is drained；
6th, crystallized stock is placed in drying cupboard drying, under the conditions of 55 DEG C, is dried to moisture less than 0.10%；7th, after drying
Material moisture it is qualified after, mix batch vanning；
8th, analytical control indices, after meeting the requirement of speciality CL-20 contract standards, packaging.
Obtained speciality CL-20 is carried out microstructure detection by the present invention, is as a result shown, the speciality that the present invention is prepared
CL-20 grain sizes are 100~110 μm, narrow particle size distribution, crystal shape rule are round and smooth.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane, comprises the following steps：
Hexanitrohexaazaisowurtzitane material solution is provided；
Stirred after the Hexanitrohexaazaisowurtzitane material solution stream is added into diluent, obtain the azepine of speciality hexanitro six
Different 5 hereby alkane；The mass ratio of solute and solvent in the Hexanitrohexaazaisowurtzitane material solution is 1：(2.5~
3.5)；The mass ratio of the diluent and solvent in the Hexanitrohexaazaisowurtzitane material solution is (1.5~1.8)：
1；The speed that the stream adds is (1.0~1.5) kg/min, and the temperature that the stream adds is 38~45 DEG C；
The particle diameter of the speciality Hexanitrohexaazaisowurtzitane is 100~110 μm；
The speed of the stirring is 500~600rpm；The diluent is low-carbon alkanes；The low-carbon alkanes are that carbon number is
6~8 alkane.
2. preparation method according to claim 1, it is characterised in that the Hexanitrohexaazaisowurtzitane material solution
In solvent be monobasic acid ester.
3. preparation method according to claim 1, it is characterised in that the temperature of the stirring is 38~45 DEG C.
4. the preparation method according to claim 1 or 3, it is characterised in that the stream adds and the total time of the stirring is 2
~3 hours.
5. preparation method according to claim 1, it is characterised in that also include after the stirring：To after the stirring
Diluent is added in feed liquid again.
6. preparation method according to claim 5, it is characterised in that the diluent added again and the hexanitro
The mass ratio of solvent is (0.1~1) in hexaazaisopen wootz alkyl material solution:1.
7. according to the preparation method any one of claim 1,5 and 6, it is characterised in that the temperature of the diluent is
38~45 DEG C.
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| CN101624394B (en) * | 2009-08-12 | 2012-09-05 | 北京理工大学 | Preparation method of sphericized hexanitrohexaazaisowurtzitane (HNIW) crystal |
| CN102898429B (en) * | 2012-09-18 | 2016-01-13 | 北京理工大学 | The recrystallization method of a kind of control ε-HNIW crystalline form and narrow size-grade distribution |
| CN103539800B (en) * | 2013-10-18 | 2015-07-29 | 中国工程物理研究院化工材料研究所 | The preparation method of macrobead Hexanitrohexaazaisowurtzitane explosive |
| CN105418619B (en) * | 2015-12-29 | 2017-12-12 | 山西北化关铝化工有限公司 | A kind of preparation method of speciality Hexanitrohexaazaisowurtzitane |
| CN105693734B (en) * | 2016-03-15 | 2018-11-09 | 北京理工大学 | A kind of speciality ε-HNIW crystal and preparation method thereof |
| CN105859730B (en) * | 2016-05-05 | 2018-05-08 | 北京理工大学 | A kind of method that anti-solvent dilution method prepares the round and smooth ε-HNIW crystal of little particle |
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