CN105503191A - Method for preparing boron carbide spray granulation powder - Google Patents

Method for preparing boron carbide spray granulation powder Download PDF

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Publication number
CN105503191A
CN105503191A CN201510929432.5A CN201510929432A CN105503191A CN 105503191 A CN105503191 A CN 105503191A CN 201510929432 A CN201510929432 A CN 201510929432A CN 105503191 A CN105503191 A CN 105503191A
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powder
granulation
norbide
boron carbide
preparation
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曹剑武
李志鹏
史秀梅
燕东明
牟晓明
李康
贾书波
杨双燕
常永威
满蓬
张武
曲俊峰
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China Weapon Science Academy Ningbo Branch
Chinese Academy of Ordnance Science Ningbo Branch
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Chinese Academy of Ordnance Science Ningbo Branch
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62695—Granulation or pelletising
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
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  • Carbon And Carbon Compounds (AREA)
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Abstract

The invention relates to a method for preparing boron carbide spray granulation powder through a spray granulation technology. The method includes the following steps that by weight, 70-80% of boron carbide powder (D50>=1 micron), 4-8% of carbon powder and 0.7-2% of yttrium oxide powder are placed in a ball mill mixing container, an adhesive agent, a dispersion agent and deionized water are added for ball milling and pulping, the rotation speed of a ball mill, the ratio of balls to materials and material mixing time are controlled, and the solid content of obtained pulp is 25-45%; the obtained pulp is introduced into a spraying drying granulation machine, and spherical granulation powder is obtained by controlling parameters such as inflow air temperature, outflow air temperature and material pump frequency. The spray granulation powder is simple in technology, low in cost, high in yield and good in granulation powder quality, and the method is suitable for preparing high-compactness and high-performance pressureless sintering boron carbide ceramics.

Description

A kind of preparation method of norbide powders by spray pelletization
Technical field
The present invention relates to a kind of method utilizing spray granulation to prepare norbide premixing flour, belong to structural ceramics field.
Technical background
Boron carbide ceramics is because having low density, high rigidity (being only second to diamond and cubic boron nitride), high elastic coefficient, corrosion-resistant, wear-resistant and absorb neutron and high temperature semiconductors characteristic, be used as neutron absorber material, bullet resistant material, wear resistant spray nozzle, semi-conductor fine structure parts etc., be used widely in fields such as nuclear energy, national defence and machineries.
Boron carbide ceramics covalent linkage mark is greater than more than 90%, and self-diffusion coefficient is very low, and the mechanism of mass transmission of the elimination of pore, crystal boundary and volume diffusion needs high temperature, and simple Sinter of Boron Carbide Ceramics is extremely difficult.At present, the preparation method having realized the high-performance boron carbide ceramics of industrialization mainly contains hot pressed sintering and pressureless sintering two kinds of techniques.Heat pressing process applies certain pressure to boron carbide sintered body sintering while, promote the densification of boron carbide ceramics, but heat pressing process list furnace output is limited, and can only the comparatively simple infrastructure product of less, the shape of preparation size, therefore hot pressing norbide comprehensive cost is very high.Non-pressure sintering technology advantage is applicable large-scale production, has low-cost advantage, and can prepare the structure unit of large size, complicated shape, is one of main preparation method of current boron carbide ceramics suitability for industrialized production.
Qualified norbide granulation powder is the important prerequisite of pressureless sintering boron carbide ceramics, and as a rule, the particle diameter of norbide granulation powder, size-grade distribution and the parameter such as mobility, moisture content directly can have influence on compact density and the sintering character of powder.
Summary of the invention
The invention provides a kind of method utilizing spray granulation to prepare norbide granulation powder, have the advantages that cost is low, output is high, superior in quality.Comprise the following steps:
(1) prepare burden: various raw material is put into mixing container, and described various raw materials comprise each component of following weight percent: boron carbide powder 70 ~ 80wt%, carbon dust 4 ~ 8wt%, yttrium oxide powder 0.7 ~ 2wt%;
(2) ball milling slurrying: add binding agent and deionized water before ball milling slurrying, the solid load of the slurry of gained is 25 ~ 45wt%.By controlling ratio of grinding media to material, drum's speed of rotation, ball mill mixing time, the obtained slurry being suitable for spray drying granulation, be specially and adopt resin, zirconium white or aluminum oxide as medium ball during ball milling, sphere diameter is 1 ~ 10mm, the ratio of the weight of ratio of grinding media to material medium ball and norbide, carbon dust, yttrium oxide powder three kinds of raw material weight sums is (0.5 ~ 5): 1, mixing time is 1 ~ 24h, and slurry pH value is 4 ~ 10, and drum's speed of rotation is 50 ~ 200 revs/min.
(3) mist projection granulating: by step (2) gained slurry, utilizes spray drying granulation technique to obtain granulation powder, is specially:
Adopt shurry pump the slurry of preparation in step (2) to be sent into atomization in the prilling spry of spray drying granulation machine and form mist droplet; the pressure of mashing pump conveying slurry is 0.02 ~ 0.4Mpa; centrifugal turntable rotating speed is 2000 ~ 20000 revs/min; the inlet temperature of spray drying granulation machine is 120 ~ 250 DEG C, temperature out 80 ~ 150 DEG C.
(4) sieve: gained powder is crossed 50-100 mesh sieve, obtain marumerizer powder, moisture content is 1-3%, and particle diameter D50 is about 70-150 μm.
Pulping equipment in above-mentioned steps of the present invention (2) is vertical or the conventional mixing equipment such as horizontal ball mill.
Purity>=95% of the boron carbide powder that the present invention is above-mentioned, particle diameter is D 50>=1 μm.
The above-mentioned carbon dust of the present invention is water colo(u)r carbon black, and particle diameter is 5 ~ 200nm.
The above-mentioned yttrium oxide powder of the present invention is purity >=95%, and particle diameter is 100nm ~ 2 μm.
Raw material in above-mentioned steps of the present invention (1) can also comprise binding agent 15 ~ 25wt%, dispersion agent 0.5 ~ 2wt%.After adding binding agent and dispersion agent, each proportioning raw materials in step (1) is: boron carbide powder 70 ~ 80wt%, carbon dust 4 ~ 8wt%, yttrium oxide powder 0.7 ~ 2wt%, binding agent 15 ~ 25wt%, dispersion agent 0.5 ~ 2wt%; Add a certain amount of deionized water before ball mill mixing, make the solid load of gained slurry be 25 ~ 45wt%.
After adding deionized water in above-mentioned steps of the present invention (2), solid load is 25 ~ 45wt%, and its solid load refers to the solid state component gross weight that boron carbide powder in raw material, yttrium oxide powder, carbon dust are formed.
The above-mentioned binding agent of the present invention can adopt in resol, polyvinyl alcohol, polyvinyl butyral acetal, methylcellulose gum one or more.
The above-mentioned dispersion agent of the present invention is one or more in ammonium polyacrylate, ammonium citrate, Tetramethylammonium hydroxide.
Advantage of the present invention and beneficial effect:
The present invention utilizes spray granulation to prepare norbide granulation powder, and particle diameter D50 is about 70-150 μm, and moisture content is about 1-3%, mobility and good forming ability, can be used for preparing high performance pressureless sintering boron carbide ceramics.Present method has that output is high, low cost and other advantages, and suitability for industrialized is produced.
Embodiment
Below by specific embodiment, the present invention is described in further detail, but the present invention is not only confined to following examples.
Raw material in the following embodiment of the present invention is commercially available prod, and equipment is industry conventional equipment.
Embodiment 1:
By boron carbide powder 900 grams of (D 50>=2 μm), carbon dust 65 grams, 10 grams, yttrium oxide powder, deionized water 2600 grams, add in ball mill mixing container, add 240g resol, 10 grams of polyvinyl alcohol and 20 grams of dispersion agents (ammonium polyacrylate) and carry out ball milling slurrying.Control ball mill mixing time, drum's speed of rotation, ratio of grinding media to material, the obtained slurry being applicable to spray drying granulation, be specially: adopt urethane ball as medium ball during ball milling, spherical diameter is 10mm, the ratio of the weight of ratio of grinding media to material and medium ball and norbide, carbon dust, yttrium oxide three kinds of raw material sums is 3:1, the ball mill mixing time is 12 hours, and slurry pH value is 8 ~ 10, and drum's speed of rotation is 80 revs/min.Then; pelletizing is obtained through mist projection granulating; be specially: after slurry being crossed 300 mesh sieves; with peristaltic pump, slurry is sent into the centrifugal turntable shower nozzle of spray drying granulation machine; the rotating speed of centrifugal turntable is 6000 revs/min; form mist droplet, the inlet temperature of spray drying granulation machine is 150 DEG C, and temperature out is 110 DEG C.Gained powder is crossed 100 mesh sieves, obtains marumerizer powder.
The moisture content of this norbide pelletizing is 1.8%, and particle diameter D50 is 110 μm, and green compact compact density is 1.45g/cm 3.
Embodiment 2:
By boron carbide powder 910 grams of (D 50>=2 μm), carbon dust 60 grams, 9 grams, yttrium oxide powder, deionized water 2500 grams, add in ball mill mixing container, add 250g resol, 10 grams of polyvinyl butyral acetals and 20 grams of dispersion agents (ammonium citrate) and carry out ball milling slurrying (ball milling pulping process is as embodiment 1).Then; pelletizing is obtained through mist projection granulating; be specially: after slurry being crossed 300 mesh sieves; with peristaltic pump, slurry is sent into the centrifugal turntable shower nozzle of spray drying granulation machine; the rotating speed of centrifugal turntable is 6000 revs/min; form mist droplet, the inlet temperature of spray drying granulation machine is 160 DEG C, and temperature out is 120 DEG C.Gained powder is crossed 100 mesh sieves, obtains marumerizer powder.
The moisture content of this norbide pelletizing is 1.6%, and particle diameter D50 is 130 μm, and green compact compact density is 1.44g/cm 3.
Embodiment 3:
By boron carbide powder 920 grams of (D 50>=2 μm), carbon dust 55 grams, 10 grams, yttrium oxide powder, deionized water 2700 grams, add in ball mill mixing container, add 250g resol, 10 grams of polyvinyl alcohol and 20 grams of dispersion agents (ammonium polyacrylate) and carry out ball milling slurrying (ball milling pulping process is as embodiment 1).Then; pelletizing is obtained through mist projection granulating; be specially: after slurry being crossed 300 mesh sieves; with peristaltic pump, slurry is sent into the centrifugal turntable shower nozzle of spray drying granulation machine; the rotating speed of centrifugal turntable is 6000 revs/min; form mist droplet, the inlet temperature of spray drying granulation machine is 150 DEG C, and temperature out is 120 DEG C.Gained powder is crossed 100 mesh sieves, obtains marumerizer powder.
The moisture content of this norbide pelletizing is 1.9%, and particle diameter D50 is 140 μm, and green compact compact density is 1.46g/cm 3.

Claims (9)

1. a preparation method for norbide granulation powder, is characterized in that: comprise the following steps:
(1) prepare burden: various raw material is put into mixing container, and described various raw materials comprise each component of following weight percent: boron carbide powder 70 ~ 80wt%, carbon dust 4 ~ 8wt%, yttrium oxide powder 0.7 ~ 2wt%;
(2) ball milling slurrying: add binding agent and deionized water before ball milling slurrying, the solid load of the slurry of gained is 25 ~ 45wt%.By controlling ratio of grinding media to material, drum's speed of rotation, ball mill mixing time, the obtained slurry being suitable for spray drying granulation, be specially and adopt resin, zirconium white or aluminum oxide as medium ball during ball milling, sphere diameter is 1 ~ 10mm, the ratio of the weight of ratio of grinding media to material medium ball and norbide, carbon dust, yttrium oxide powder three kinds of raw material weight sums is (0.5 ~ 5): 1, mixing time is 1 ~ 24h, and slurry pH value is 4 ~ 10, and drum's speed of rotation is 50 ~ 200 revs/min.
(3) mist projection granulating: by step (2) gained slurry, utilizes spray drying granulation technique to obtain granulation powder, is specially:
Adopt shurry pump the slurry of preparation in step (2) to be sent into atomization in the prilling spry of spray drying granulation machine and form mist droplet; the pressure of mashing pump conveying slurry is 0.02 ~ 0.4Mpa; centrifugal turntable rotating speed is 2000 ~ 20000 revs/min; the inlet temperature of spray drying granulation machine is 120 ~ 250 DEG C, temperature out 80 ~ 150 DEG C.
(4) sieve: gained powder is crossed 50-100 mesh sieve, obtain marumerizer powder, moisture content is 1-3%, and particle diameter D50 is about 70-150 μm.
2. the preparation method of norbide granulation powder according to claim 1, is characterized in that: the pulping equipment in step (1) is vertical or horizontal ball mill.
3. the preparation method of norbide granulation powder according to claim 1, it is characterized in that: the ball milling slurrying in step (1), by controlling ratio of grinding media to material, drum's speed of rotation, the ball mill mixing time, the obtained slurry being suitable for spray drying granulation, be specially employing resin, zirconium white or aluminum oxide are as medium ball during ball milling, sphere diameter is 1 ~ 10mm, the weight of ratio of grinding media to material and medium ball and norbide, carbon dust, the ratio of yttrium oxide powder three kinds of raw material weight sums is (0.5 ~ 5): 1, mixing time is 1 ~ 24h, slurry pH value is 4 ~ 10, drum's speed of rotation is 50 ~ 900 revs/min.
4. the preparation method of norbide granulation powder according to claim 1, is characterized in that: described boron carbide powder is purity>=95%, and median size is D 50the boron carbide powder of>=1 μm.
5. the preparation method of norbide granulation powder according to claim 1, is characterized in that: described carbon dust is water colo(u)r carbon black, and particle diameter is 5 ~ 200nm.
6. the pressureless sintering boron carbide ceramics preparation method based on coarse particles powder according to claim 1, is characterized in that: described yttrium oxide powder purity >=95%, particle diameter is 100nm ~ 2 μm.
7. the preparation method of norbide granulation powder according to claim 1, it is characterized in that the raw material in step (1) can also comprise binding agent and dispersion agent, after adding binding agent and dispersion agent, each proportioning raw materials in step (1) is: boron carbide powder 70 ~ 80wt%, carbon dust 4 ~ 8wt%, yttrium oxide powder 0.7 ~ 2wt%, binding agent 15 ~ 25wt%, dispersion agent 0.5 ~ 2wt%; Add a certain amount of deionized water before ball mill mixing, make the solid load of gained slurry be 25 ~ 45wt%.
8. the preparation method of norbide granulation powder according to claim 7, is characterized in that: described binding agent is one or more in resol, polyvinyl alcohol, polyvinyl butyral acetal, methylcellulose gum.
9. the preparation method of norbide granulation powder according to claim 7, is characterized in that: described dispersion agent is one or more in ammonium polyacrylate, ammonium citrate, Tetramethylammonium hydroxide.
CN201510929432.5A 2015-12-15 2015-12-15 Method for preparing boron carbide spray granulation powder Pending CN105503191A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106278273A (en) * 2016-08-30 2017-01-04 大连正兴磨料有限公司 A kind of preparation method of superfine boron carbide mist projection granulating powder
CN106631009A (en) * 2016-10-14 2017-05-10 河北工业大学 Composite powder for zirconium boride based composite material and preparation method of composite powder
CN110368918A (en) * 2019-08-15 2019-10-25 西南化工研究设计院有限公司 A kind of Spray granulation method of boehmite powder
CN110883337A (en) * 2019-12-04 2020-03-17 电子科技大学 Spray granulation Fe-Al2O3Preparation method of spraying composite powder
CN111848169A (en) * 2020-07-10 2020-10-30 沈阳和世泰通用钛业有限公司 Ceramic and preparation method and application thereof
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
CN112194491A (en) * 2020-10-15 2021-01-08 山东亚赛陶瓷科技有限公司 Pressureless sintering boron carbide ceramic powder and preparation method and application thereof
CN112226720A (en) * 2020-10-15 2021-01-15 电子科技大学 Spray granulation preparation method of metal-ceramic composite powder suitable for atmospheric plasma spraying
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

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106278273A (en) * 2016-08-30 2017-01-04 大连正兴磨料有限公司 A kind of preparation method of superfine boron carbide mist projection granulating powder
CN106631009A (en) * 2016-10-14 2017-05-10 河北工业大学 Composite powder for zirconium boride based composite material and preparation method of composite powder
CN106631009B (en) * 2016-10-14 2019-07-30 河北工业大学 A kind of composite powder and preparation method thereof for boronation zirconium based composite material
CN110368918A (en) * 2019-08-15 2019-10-25 西南化工研究设计院有限公司 A kind of Spray granulation method of boehmite powder
CN110883337A (en) * 2019-12-04 2020-03-17 电子科技大学 Spray granulation Fe-Al2O3Preparation method of spraying composite powder
CN111848169A (en) * 2020-07-10 2020-10-30 沈阳和世泰通用钛业有限公司 Ceramic and preparation method and application thereof
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
CN112079642B (en) * 2020-08-17 2022-09-23 沈阳中钛装备制造有限公司 Boron carbide spray granulation powder and preparation method and application thereof
CN112194491A (en) * 2020-10-15 2021-01-08 山东亚赛陶瓷科技有限公司 Pressureless sintering boron carbide ceramic powder and preparation method and application thereof
CN112226720A (en) * 2020-10-15 2021-01-15 电子科技大学 Spray granulation preparation method of metal-ceramic composite powder suitable for atmospheric plasma spraying
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
CN112830798B (en) * 2021-01-19 2022-05-06 哈尔滨工业大学 Preparation method of boron carbide granulation powder for pressureless sintering

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Application publication date: 20160420