CN107117971A - A kind of method that high-energy ball milling combination spray drying technology prepares superfine boron carbide pelletizing - Google Patents

A kind of method that high-energy ball milling combination spray drying technology prepares superfine boron carbide pelletizing Download PDF

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CN107117971A
CN107117971A CN201710272252.3A CN201710272252A CN107117971A CN 107117971 A CN107117971 A CN 107117971A CN 201710272252 A CN201710272252 A CN 201710272252A CN 107117971 A CN107117971 A CN 107117971A
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ball
boron carbide
binding agent
ball milling
spray drying
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王为民
许晓晖
何强龙
王爱阳
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—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
    • 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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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62695—Granulation or pelletising
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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Abstract

The present invention relates to a kind of method that high-energy ball milling combination spray drying technology prepares superfine boron carbide pelletizing, its step is as follows：1) dispensing；2) slurrying：Deionized water, lubricant A, lubricant B, dispersant, binding agent A, binding agent B are placed in polytetrafluoroethylene (PTFE) ball grinder, addition ball milling ball, which is placed on planetary ball mill, carries out ball mill mixing, then boron carbide micro powder is added in ball grinder, continue ball milling 0.5h, binding agent C is added into 12~18h of ball milling in ball grinder again, defoamer finally is added into ball milling 10min in ball grinder obtains slurry；3) spray drying granulation：Granulation is dried with spray drying granulation instrument in slurry, superfine boron carbide pelletizing is obtained.The present invention obtains spherical granulation powder using wet method high-energy ball milling combination atomizing granulating technology, and gained powder contributes to the shaping of boron carbide powder, improves the relative density of biscuit.

Description

A kind of high-energy ball milling combination spray drying technology prepares superfine boron carbide pelletizing Method
Technical field
The present invention relates to the preparation method of powder body material, and in particular to prepared by a kind of high-energy ball milling combination spray drying technology The method of superfine boron carbide pelletizing.
Background technology
Boron carbide has higher B-C covalent bonds and relatively low self-diffusion coefficient.Extremely strong covalent bond imparts boron carbide The excellent performance of ceramics, such as：The hardness and wearability of superelevation, high-melting-point etc..But its sintering character is reduced again simultaneously, increase The difficulty of sintering densification.
Pressureless sintering method can prepare large scale, the various products of complex contour with relatively low cost, be adapted to high-volume Production, with industrial prospect.But boron carbide covalent bond is extremely strong, self-diffusion coefficient is very low, crystal boundary movement is difficult, and pressureless sintering is caused Densification is difficult, and such as conventional boron carbide pellet can only achieve 80% or so consistency using pressureless sintering.The grain of boron carbide powder The parameters such as footpath size, size distribution and mobility can directly influence the compact density and sintering character of powder, can be by subtracting Small powder size helps to sinter, but powder is meticulous, such as thin to submicron order or nanoscale, then the specific surface area of powder granule compared with Greatly, specific surface energy is high, is very easy to reunite, the mobility of powder granule is very poor, dispersiveness is also bad.Using material by wet type mixing-spray The technique of mist granulation can avoid the reunion again and sedimentation of the component of each in slurry, and obtained slurry dispersion stabilization is good, And the granulated pellet obtained by spray drying is shaped as spherical, size distribution level is with reasonable, and mobile performance is good, by powder spray Obtained biscuit consistency is suppressed after granulation and uniformity is greatly improved, is conducive to the pressureless sintering of boron carbide ceramics.
Existing spray granulation typically uses the ceramic raw material of certain crystal particle scale, addition various functions additive, After organic solvent such as ethanol, the dispersed of ceramic powder and additive is realized by normal wet ball milling, then be spray-dried Granulation.It is spray-dried using organic solvent, not only cost is high and there is safety problem, develops the mist projection granulating of aqueous based systems slurry Technology turns into the inexorable trend of ceramic slurry mist projection granulating, but is applied to also need to further improve correlation in boron carbide ceramics Technology.
The content of the invention
The technical problems to be solved by the invention are that there is provided a kind of high energy ball for above shortcomings in the prior art The method that mill prepares superfine boron carbide pelletizing with reference to spray drying technology, using deionized water as solvent, gained superfine boron carbide Pelletizing mobility is greatly improved, and processability is good, and the crystal particle scale for obtaining biscuit significantly reduces, uniformity and compactness are carried Height, suitably manufactures the high performance boron carbide ceramics of high-compactness.
In order to solve the above technical problems, the technical scheme that the present invention is provided is：
A kind of method that high-energy ball milling combination spray drying technology prepares superfine boron carbide pelletizing is provided, its step is such as Under：
1) dispensing：By each raw material according to following mass percent dispensing：Boron carbide micro powder 45~51%, deionized water 38~ 45%, lubricant A 0.9~1%, lubricant B 0.45~0.51%, dispersant 0.45~0.51%, binding agent A 2.3~ 2.6%, binding agent B 0.45~0.51%, binding agent C 4.5~5.1%, defoamer 0.04~0.07%；
2) slurrying：Deionized water, lubricant A, lubricant B, dispersant, binding agent A, binding agent B are placed in polytetrafluoroethyl-ne In alkene ball grinder, addition ball milling ball, which is placed on planetary ball mill, carries out ball mill mixing, and boron carbide micro powder then is added into ball grinder In, continue ball milling 0.5h, then binding agent C is added into 12~18h of ball milling in ball grinder, defoamer is finally added into ball in ball grinder Mill 10min obtains slurry；
3) spray drying granulation：By step 2) gained slurry granulation is dried with spray drying granulation instrument, obtain ultra-fine Boron carbide pelletizing.
By such scheme, step 1) the median D of the boron carbide micro powder50For 2.5~3.5 μm.
By such scheme, step 1) the lubricant A be polyoxyethylene series lubricant agent；The lubricant B is glycerine；It is described Dispersant is ammonia alcohols dispersant；The binding agent A is polyvinyl alcohol binding agent；The binding agent B is cyclodextrin；It is described viscous It is water soluble phenol resin to tie agent C；The defoamer is propane diols.
By such scheme, step 2) technique of the ball mill mixing is：Ball milling ball use boron carbide ball, ratio of grinding media to material be 3~ 4:1, rotational speed of ball-mill is 300r/min, and Ball-milling Time is 0.5h.
By such scheme, step 3) process conditions of the spray drying granulation are：Spray drying granulation instrument inlet temperature For 175~185 DEG C, outlet temperature is 90~105 DEG C, and pump speed is 8%, and air mass flow is 45~60m3/h。
Present invention additionally comprises the superfine boron carbide pelletizing prepared according to the above method, the superfine boron carbide pelletizing is Regular spherical, median D50For 50~130 μm, superfine boron carbide pelletizing is by uniform boron carbide powder particle packing Form, the median D of boron carbide powder particle50For 0.8~1.2 μm.
High energy wet ball grinding not only can also can simultaneously refine ceramic particle grain with dispersed ceramic powder and additive Footpath, obtains the dispersed system of crystal grain refinement.Mist projection granulating is that powder is carried out to be spray-dried after fluidization processing, will be mixed Good slurry Direct spraying is dried within the very short time into hot-air, obtains the spherical powder of regular shape.To ceramics Slurry application atomizing granulating technology, can avoid reuniting again and sedimentation separation for each component, maintain the original uniformity of slurry； Slurry atomization is uniform simultaneously, and obtained powder granularity is evenly distributed, good fluidity, is adapted to continuous automatic moulding, improves efficiency, subtracts Few dust, shortens the time of people's manual contact powder, and is conducive to improving density, uniformity and the sintering character of biscuit.
The beneficial effects of the present invention are：The present invention uses wet method high-energy ball milling combination atomizing granulating technology, by average grain The business boron carbide powder ball milling refinement granulation in 2.5~3.5 μm of footpath, is obtained in the regular smooth ultra-fine carbon in regular spherical, surface Change under boron pelletizing, different technology conditions, the D of pelletizing50It is generally between 50~130 μm, pelletizing is homogeneous, near by size Spheroidal boron carbide powder particle packing is formed, the median D of boron carbide powder particle50For 0.8~1.2 μm.Pelletizing 0.72~0.84g/cm of body apparent density3, angle of repose is at 20~26 °；By pelletizing dry-pressing under 40~50MPa briquetting pressure Shaping, then after isostatic cool pressing under 200MPa, obtained biscuit density is in 1.4~1.9g/cm3, with the former micro mist phase of boron carbide Than apparent density improves more than 50%, and angle of repose also significantly reduces, and the relative density of biscuit is up to 59%.To sum up may be used Know, by mist projection granulating handle powder processing performance be improved significantly, it is high to obtain biscuit density, suitably prepares high-compactness High performance boron carbide ceramics.
Brief description of the drawings
Fig. 1 is the SEM figures of the superfine boron carbide pelletizing prepared by embodiment 1；
Fig. 2 is the SEM figures of the superfine boron carbide pelletizing prepared by embodiment 2；
Fig. 3 is the SEM figures of the superfine boron carbide pelletizing prepared by embodiment 3.
Embodiment
To make those skilled in the art more fully understand technical scheme, the present invention is made below in conjunction with the accompanying drawings into One step is described in detail.
The embodiment of the present invention with lubricator A be Wuhan Mei Qilin new materials Co., Ltd produce polyoxyethylene-modified system Agent MQ9002；Dispersant used is the ammonia alcohol compound MQ5088 that Wuhan Mei Qilin new materials Co., Ltd produces；Bonding used Agent A is the modified polyvinylalcohol product MQ35 that Wuhan Mei Qilin new materials Co., Ltd produces.
Embodiment 1
By each raw material according to following mass percent dispensing：Boron carbide micro powder 20g (D50：2.5~3.5 μm), deionized water 20g, lubricant A 0.4g, glycerine 0.2g, dispersant 0.2g, binding agent A 1g, cyclodextrin 0.2g, water soluble phenol resin 2g, Propane diols 0.02g；
Deionized water, lubricant A, glycerine, dispersant, binding agent A, cyclodextrin are placed in polytetrafluoroethylene (PTFE) ball grinder, Addition boron carbide ball, which is placed on planetary ball mill, carries out ball mill mixing, and ratio of grinding media to material is 3:1, rotational speed of ball-mill is 300r/min, ball milling 0.5h, then adds boron carbide micro powder in ball grinder, continues ball milling 0.5h, then water soluble phenol resin is added in ball grinder Ball milling 12h, finally adds ball milling 10min in ball grinder by propane diols and obtains slurry；Gained slurry spray drying granulation instrument enters Row drying-granulating, 180 DEG C of setting spray drying granulation instrument inlet temperature, 90~105 DEG C of outlet temperature, pump speed is 8%, air stream Measure as 45~60m3Pelletizing is collected in/h, cooling, is crossed 300 mesh sieves, is obtained superfine boron carbide pelletizing.
After tested, the viscosity of the slurry obtained by the present embodiment is the Zeta potential of boron carbide particles in 20mpas, slurry For -68mV, illustrate that the viscosity of gained slurry is low, dispersion stabilization is good, measure the medians of boron carbide particles in slurry between Between 0.8~1.2 μm.The scanning electron microscope (SEM) photograph of pelletizing is as shown in Figure 1 obtained by the present embodiment, it is seen that powder is spherical in rule, makes Grain powder surface is regular smooth, and the particle diameter distribution for granulating powder particles is larger, and size diameter is between 30~150 μm.Granulation powder pine is filled out Density is filled for 0.72g/cm3, angle of repose is 22 °, pelletizing is carried out under 43MPa dry-pressing formed, is then entered under 200MPa After row cold isostatic compaction, the density for measuring biscuit is 1.43g/cm3(boron carbide micro powder density is 2.52g/cm3), relative density For 57%.
Embodiment 2
By each raw material according to following mass percent dispensing：Boron carbide micro powder 20g (D50：2.5~3.5 μm), deionized water 18g, lubricant A 0.4g, glycerine 0.2g, dispersant 0.2g, binding agent A 1g, cyclodextrin 0.2g, water soluble phenol resin 2g, Propane diols 0.02g；
Deionized water, lubricant A, glycerine, dispersant, binding agent A, cyclodextrin are placed in polytetrafluoroethylene (PTFE) ball grinder, Addition boron carbide ball, which is placed on planetary ball mill, carries out ball mill mixing, and ratio of grinding media to material is 4:1, rotational speed of ball-mill is 300r/min, ball milling 0.5h, then adds boron carbide micro powder in ball grinder, continues ball milling 0.5h, then water soluble phenol resin is added in ball grinder Ball milling 18h, finally adds ball milling 10min in ball grinder by propane diols and obtains slurry；Gained slurry spray drying granulation instrument enters Row drying-granulating, 175 DEG C of setting spray drying granulation instrument inlet temperature, 90~105 DEG C of outlet temperature, pump speed is 8%, air stream Measure as 45~60m3Pelletizing is collected in/h, cooling, is crossed 300 mesh sieves, is obtained superfine boron carbide pelletizing.
After tested, the viscosity of the slurry obtained by the present embodiment is the Zeta potential of boron carbide particles in 25mpas, slurry For -65mV, illustrate that the viscosity of gained slurry is low, dispersion stabilization is good, measure the medians of boron carbide particles in slurry between Between 0.8~1.0 μm.Gained pelletizing scanning electron microscope (SEM) photograph is as shown in Figure 2, it is seen that powder is spherical in rule, pelletizing surface rule Whole smooth, the particle diameter distribution for granulating powder particles is larger, and size diameter is between 50~150 μm.Granulation powder pine packed density be 0.8g/cm3, angle of repose is 20 °, pelletizing is carried out under 43MPa dry-pressing formed, and isostatic cool pressing is then carried out under 200MPa After shaping, the density for measuring biscuit is 1.45g/cm3, relative density is 58%.
Embodiment 3
By each raw material according to following mass percent dispensing：Boron carbide micro powder 20g (D50：2.5~3.5 μm), deionized water 15g, lubricant A 0.4g, glycerine 0.2g, dispersant 0.2g, binding agent A 1g, cyclodextrin 0.2g, water soluble phenol resin 2g, Propane diols 0.02g；
Deionized water, lubricant A, glycerine, dispersant, binding agent A, cyclodextrin are placed in polytetrafluoroethylene (PTFE) ball grinder, Addition boron carbide ball, which is placed on planetary ball mill, carries out ball mill mixing, and ratio of grinding media to material is 4:1, rotational speed of ball-mill is 300r/min, ball milling 0.5h, then adds boron carbide micro powder in ball grinder, continues ball milling 0.5h, then water soluble phenol resin is added in ball grinder Ball milling 18h, finally adds ball milling 10min in ball grinder by propane diols and obtains slurry；Gained slurry spray drying granulation instrument enters Row drying-granulating, 185 DEG C of setting spray drying granulation instrument inlet temperature, 90~105 DEG C of outlet temperature, pump speed is 8%, air stream Measure as 45~60m3Pelletizing is collected in/h, cooling, is crossed 300 mesh sieves, is obtained superfine boron carbide pelletizing.
After tested, the viscosity of the slurry obtained by the present embodiment is the Zeta potential of boron carbide particles in 28mpas, slurry For -62mV, illustrate that the viscosity of gained slurry is low, dispersion stabilization is good, measure the medians of boron carbide particles in slurry between Between 0.8~1.0 μm.Gained pelletizing scanning electron microscope (SEM) photograph is as shown in Figure 3, it is seen that powder is spherical in rule, pelletizing surface rule Whole smooth, the particle diameter distribution for granulating powder particles is larger, and size diameter is between 50~150 μm.Granulation powder pine packed density be 0.84g/cm3, angle of repose is 20 °, pelletizing is carried out under 43MPa dry-pressing formed, is then carried out under 200MPa cold etc. quiet After molded, the density for measuring biscuit is 1.48g/cm3, relative density is 59%.

Claims (6)

1. a kind of method that high-energy ball milling combination spray drying technology prepares superfine boron carbide pelletizing, it is characterised in that step It is as follows：
1) dispensing：By each raw material according to following mass percent dispensing：Boron carbide micro powder 45~51%, deionized water 38~ 45%, lubricant A 0.9~1%, lubricant B 0.45~0.51%, dispersant 0.45~0.51%, binding agent A 2.3~ 2.6%, binding agent B 0.45~0.51%, binding agent C 4.5~5.1%, defoamer 0.04~0.07%；
2) slurrying：Deionized water, lubricant A, lubricant B, dispersant, binding agent A, binding agent B are placed in polytetrafluoroethylene (PTFE) ball In grinding jar, addition ball milling ball, which is placed on planetary ball mill, carries out ball mill mixing, then adds boron carbide micro powder in ball grinder, after Continuous ball milling 0.5h, then binding agent C is added into 12~18h of ball milling in ball grinder, defoamer is finally added into ball milling in ball grinder 10min obtains slurry；
3) spray drying granulation：By step 2) gained slurry granulation is dried with spray drying granulation instrument, obtain ultra-fine carbonization Boron pelletizing.
2. according to the method described in claim 1, it is characterised in that：Step 1) boron carbide micro powder median D50For 2.5~3.5 μm.
3. according to the method described in claim 1, it is characterised in that：Step 1) the lubricant A be polyoxyethylene series lubricant agent； The lubricant B is glycerine；The dispersant is ammonia alcohols dispersant；The binding agent A is polyvinyl alcohol binding agent；It is described Binding agent B is cyclodextrin；The binding agent C is water soluble phenol resin；The defoamer is propane diols.
4. the technique of the ball mill mixing is according to the method described in claim 1, it is characterised in that step 2)：Ball milling ball is adopted Boron carbide ball is used, ratio of grinding media to material is 3~4:1, rotational speed of ball-mill is 300r/min, and Ball-milling Time is 0.5h.
5. the process conditions of the spray drying granulation are according to the method described in claim 1, it is characterised in that step 3)： Spray drying granulation instrument inlet temperature is 175~185 DEG C, and outlet temperature is 90~105 DEG C, and pump speed is 8%, and air mass flow is 45 ~60m3/h。
6. a kind of superfine boron carbide pelletizing prepared according to any methods describeds of claim 1-5, it is characterised in that：It is described super Thin boron carbide pelletizing is regular spherical, median D50For 50~130 μm, superfine boron carbide pelletizing is by uniform carbon Change boron powder particle packing to form, the median D of boron carbide powder particle50For 0.8~1.2 μm.
CN201710272252.3A 2017-04-24 2017-04-24 A kind of method that high-energy ball milling combination spray drying technology prepares superfine boron carbide pelletizing Pending CN107117971A (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN108911754A (en) * 2018-09-29 2018-11-30 吉林长玉特陶新材料技术股份有限公司 A kind of normal pressure-sintered method for preparing boron carbide ceramics of dry method
CN110883337A (en) * 2019-12-04 2020-03-17 电子科技大学 Spray granulation Fe-Al2O3Preparation method of spraying composite powder
CN112079642A (en) * 2020-08-17 2020-12-15 沈阳中钛装备制造有限公司 Boron carbide spray granulation powder and preparation method and application thereof
CN112830798A (en) * 2021-01-19 2021-05-25 黑龙江冠瓷科技有限公司 Preparation method of boron carbide granulation powder for pressureless sintering
CN114538929A (en) * 2022-03-17 2022-05-27 南通三责精密陶瓷有限公司 Preparation method of high-density boron carbide ceramic
CN114669749A (en) * 2022-04-01 2022-06-28 西安西电高压开关有限责任公司 Preparation system and method of high-performance superfine contact material
CN116161960A (en) * 2022-12-31 2023-05-26 宁波伏尔肯科技股份有限公司 Superfine boron carbide casting slurry and preparation method of ceramic thereof

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