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CN108530066A - A kind of manufacturing method of high purity niobium oxide ontology crucible - Google Patents

A kind of manufacturing method of high purity niobium oxide ontology crucible Download PDF

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Publication number
CN108530066A
CN108530066A CN201810314735.XA CN201810314735A CN108530066A CN 108530066 A CN108530066 A CN 108530066A CN 201810314735 A CN201810314735 A CN 201810314735A CN 108530066 A CN108530066 A CN 108530066A
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Prior art keywords
niobium oxide
high purity
crucible
purity niobium
minutes
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CN201810314735.XA
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Chinese (zh)
Inventor
张和鹏
张镇
张�浩
戴和平
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JIUJIANG NONFERROUS METAL SMELTING CO Ltd
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JIUJIANG NONFERROUS METAL SMELTING CO Ltd
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Priority to CN201810314735.XA priority Critical patent/CN108530066A/en
Publication of CN108530066A publication Critical patent/CN108530066A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66Monolithic refractories or refractory mortars, including those whether or not containing clay
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B3/00Producing shaped articles from the material by using presses; Presses specially adapted therefor
    • B28B3/003Pressing by means acting upon the material via flexible mould wall parts, e.g. by means of inflatable cores, isostatic presses
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/495Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/6261Milling
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing 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
    • C04B35/632Organic additives
    • C04B35/634Polymers
    • C04B35/63404Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63416Polyvinylalcohols [PVA]; Polyvinylacetates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607Thermal properties, e.g. thermal expansion coefficient

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Powder Metallurgy (AREA)

Abstract

A kind of manufacturing method of high purity niobium oxide ontology crucible, the technical solution of the manufacturing method are:High purity niobium oxide powder is by dispensing, granulation, compacting, drying, high temperature sintering, annealing, polishing, finished product.This method rational technology, manufacturing cost are low, products obtained therefrom intensity is high, purity is good, water absorption rate is low, good thermal shock, deformation are small, substantially without cracking the defects of, service life is long, durability is high.

Description

A kind of manufacturing method of high purity niobium oxide ontology crucible
Technical field
The present invention relates to a kind of manufacturing methods of high purity niobium oxide ontology crucible.
Background technology
At present the production method of niobium oxide ontology crucible mainly have slip casting, injection moulding or injection moulding, etc. it is quiet Molded method etc..Slip casting is that plaster mold water suction is leaned on to realize completely, has density gradient distribution in green body, is easily formed not Homogeneous deformation, it is difficult to obtain the product of high intensity, high-purity.Injection moulding or injection moulding need to be added a certain amount of paraffin and cause Skimming processes are cumbersome, and production cost is high, and the thawing or evaporation of bonding agent make the strength reduction of green body, easily form defect and even open It splits, collapse.Isostatic pressing method has intensity height, does not introduce impurity, the product purity of effective guarantee calcining.
Invention content
Its purpose of the invention, which is that, provides a kind of manufacturing method of high purity niobium oxide ontology crucible, solves the prior art It is cumbersome that there are processes, and production cost is high, and the thawing or evaporation of bonding agent make the strength reduction of green body, easily forms defect and even opens The problem of splitting, collapsing.
It adopts the technical scheme that, a kind of manufacturing method of high purity niobium oxide ontology crucible, wraps to achieve the above object Include following steps:
1), high purity niobium oxide powder is allocated, amount of preparation based on 100kg, wherein:60% ~ 70% high purity niobium oxide, 20% ~ 25% ultra-pure water, 10% ~ 15% bonding agent, bonding agent PVA contents 5% ~ 10% add 100mL ~ 300mL dispersants, and dispersant is A135 is put into 300L wet milks;
2), niobium alloy ball 30 kg ~ 40kg, ratio of grinding media to material 1 is added:2.5~3.5;
3), powders mixture ball milling 2 hours, after taking slurries to cross 500 ~ 800 mesh sieve, spray drying obtains mobility and is less than 150 seconds Nearly ball-type high purity niobium oxide particle;
4), take 1.4kg ~ 1.5kg granulation high purity niobium oxide is fitted into rubber mold, rubber die lock, prevent leak;
5), the mold that will feed be put into isostatic pressed cylinder body, slowly boost to 100 ~ 110 megapascal within 15 minutes, then slowly decompression To 70 ~ 75 megapascal pressurize 5 minutes, it is down to 50 ~ 55 megapascal pressurize 5 minutes, is down to 15 ~ 20 megapascal pressurize 5 minutes, then is down to often Pressure;
6), open isostatic pressed cylinder cap, take out compacting tool set, carefully dismantle rubber pattern, take out the high purity niobium oxide crucible suppressed Green body;
7), crucible green body is packed into baking oven, be warming up to 100 DEG C ~ 150 DEG C, keep the temperature 24 hours, be cooled to room temperature, be packed into high temperature and burn Freezing of a furnace;
8), the crucible green body of drying is upside down in high temperature sintering furnace body, propped up with corundum tablet, prevent from deforming, be spilt on tablet Upper niobium oxide powder, haftplatte when preventing high temperature sintering;
9), high temperature sintering furnace heating process it is as follows:50 DEG C every liter keep the temperature 30 minutes, are raised to 1300 DEG C ~ 1350 DEG C always, heat preservation 2 Hour, it cools to room temperature with the furnace, comes out of the stove;
10), polishing, packaging and storage.
Advantageous effect
The present invention has the following advantages compared with prior art.
It is an advantage of the invention that this method rational technology, manufacturing cost are low, products obtained therefrom intensity is high, purity is good, water absorption rate Low, good thermal shock, deformation be small, substantially without cracking the defects of, service life is long, durability is high.
Specific implementation mode
A kind of manufacturing method of high purity niobium oxide ontology crucible, includes the following steps:
1), high purity niobium oxide powder is allocated, amount of preparation based on 100kg, wherein:60% ~ 70% high purity niobium oxide, 20% ~ 25% ultra-pure water, 10% ~ 15% bonding agent, bonding agent PVA contents 5% ~ 10% add 100mL ~ 300mL dispersants, and dispersant is A135 is put into 300L wet milks;
2), niobium alloy ball 30 kg ~ 40kg, ratio of grinding media to material 1 is added:2.5~3.5;
3), powders mixture ball milling 2 hours, after taking slurries to cross 500 ~ 800 mesh sieve, spray drying obtains mobility and is less than 150 seconds Nearly ball-type high purity niobium oxide particle;
4), take 1.4kg ~ 1.5kg granulation high purity niobium oxide is fitted into rubber mold, rubber die lock, prevent leak;
5), the mold that will feed be put into isostatic pressed cylinder body, slowly boost to 100 ~ 110 megapascal within 15 minutes, then slowly decompression To 70 ~ 75 megapascal pressurize 5 minutes, it is down to 50 ~ 55 megapascal pressurize 5 minutes, is down to 15 ~ 20 megapascal pressurize 5 minutes, then is down to often Pressure;
6), open isostatic pressed cylinder cap, take out compacting tool set, carefully dismantle rubber pattern, take out the high purity niobium oxide crucible suppressed Green body;
7), crucible green body is packed into baking oven, be warming up to 100 DEG C ~ 150 DEG C, keep the temperature 24 hours, be cooled to room temperature, be packed into high temperature and burn Freezing of a furnace;
8), the crucible green body of drying is upside down in high temperature sintering furnace body, propped up with corundum tablet, prevent from deforming, be spilt on tablet Upper niobium oxide powder, haftplatte when preventing high temperature sintering;
9), high temperature sintering furnace heating process it is as follows:50 DEG C every liter keep the temperature 30 minutes, are raised to 1300 DEG C ~ 1350 DEG C always, heat preservation 2 Hour, it cools to room temperature with the furnace, comes out of the stove;
10), polishing, packaging and storage.
Embodiment one:
1, high purity niobium oxide powder is allocated, amount of preparation 100kg meters, wherein 66% high purity niobium oxide, 22% ultra-pure water, 12% Bonding agent(PVA contents 5%), add 300mL dispersants(A135)Solution is put into 300L wet milks;
2, niobium alloy ball 40kg is added;
3, powders mixture ball milling 2 hours carry out spray drying granulation after taking slurries to cross 500 mesh sieve, obtain mobility and are less than 130 seconds nearly ball-type high purity niobium oxide particles;
4,1.5kg granulation high purity niobium oxides are taken to be fitted into mold, rubber die locking prevents leak;
5, the mold that will feed is put into isostatic pressed cylinder body, is slowly boosted to 105 megapascal within 15 minutes, is then slowly depressurized to 75,000,000 50 megapascal pressurize 5 minutes is down in pa pressurize 5 minutes, is down to 18 megapascal pressurize 5 minutes, then be down to normal pressure;
6, isostatic pressed cylinder cap is opened, mold is taken out, dismantles rubber pattern, take out the crucible green body suppressed;
7, crucible green body is packed into baking oven, is warming up to 105 DEG C, kept the temperature 24 hours, be cooled to room temperature, be packed into high temperature sintering furnace.
8, the crucible green body of drying is upside down in high temperature sintering furnace body, is propped up with corundum tablet, prevent from deforming, on tablet It is sprinkled with niobium oxide powder, haftplatte when preventing from being sintered;
9, high temperature sintering furnace heating process is as follows:50 DEG C every liter keep the temperature 30 minutes, are raised to 1330 DEG C always, 2 hours are kept the temperature, with stove It is cooled to room temperature.
10, it polishes, packaging and storage.
One high purity niobium oxide ontology crucible performance parameter of embodiment is as follows:
Coefficient of thermal expansion:1.45×10-6/ K;
Water absorption rate:2%;
Purity:99.99%;
Flexural strength:12.1Mpa;
Deformation rate:Less than 1%;
Heat rate:More than 1000 times.
Embodiment two:
1, high purity niobium oxide powder is allocated, 67% high purity niobium oxide, 23% ultra-pure water, 10% bonding agent(PVA contents 6%), Add 250mL dispersants(A135)Solution is put into 300L wet milks;
2, niobium alloy ball 40kg is added;
3, powders mixture ball milling 2 hours carry out spray drying granulation after taking slurries to cross 500 mesh sieve, obtain mobility and are less than 100 seconds nearly ball-type high purity niobium oxide particles;
4,1.45kg granulation high purity niobium oxides are taken to be fitted into mold, rubber die locking prevents leak;
5, the mold that will feed is put into isostatic pressed cylinder body, is slowly boosted to 105 megapascal within 5 minutes, is then slowly depressurized to 75,000,000 Pa pressurize 3 minutes is down to 50 megapascal pressurize 2 minutes, then is down to normal pressure;
6, isostatic pressed cylinder cap is opened, mold is taken out, dismantles rubber pattern, take out the crucible green body suppressed;
7, crucible green body is packed into baking oven, is warming up to 120 DEG C, kept the temperature 24 hours, be cooled to room temperature, be packed into high temperature sintering furnace.
8, the crucible green body of drying is upside down in furnace body, is propped up with corundum tablet, prevent from deforming, oxidation is sprinkled on tablet Niobium powder, haftplatte when preventing from being sintered;
9, high temperature sintering furnace heating process is as follows:50 DEG C every liter keep the temperature 30 minutes, are raised to 1350 DEG C always, 2 hours are kept the temperature, with stove It is cooled to room temperature,
10, it polishes, packaging and storage.
Two high purity niobium oxide ontology crucible performance parameter of embodiment is as follows:
Coefficient of thermal expansion:1.45×10-6/ K;
Water absorption rate:1.5%;
Purity:99.99%;
Flexural strength:13.1Mpa;
Deformation rate:Less than 1%;
Heat rate:More than 1000 times.

Claims (1)

1. a kind of manufacturing method of high purity niobium oxide ontology crucible, which is characterized in that include the following steps:
1), high purity niobium oxide powder is allocated, amount of preparation based on 100kg, wherein:60% ~ 70% high purity niobium oxide, 20% ~ 25% ultra-pure water, 10% ~ 15% bonding agent, bonding agent PVA contents 5% ~ 10% add 100mL ~ 300mL dispersants, and dispersant is A135 is put into 300L wet milks;
2), niobium alloy ball 30 kg ~ 40kg, ratio of grinding media to material 1 is added:2.5~3.5;
3), powders mixture ball milling 2 hours, after taking slurries to cross 500 ~ 800 mesh sieve, spray drying obtains mobility and is less than 150 seconds Nearly ball-type high purity niobium oxide particle;
4), take 1.4kg ~ 1.5kg granulation high purity niobium oxide is fitted into rubber mold, rubber die lock, prevent leak;
5), the mold that will feed be put into isostatic pressed cylinder body, slowly boost to 100 ~ 110 megapascal within 15 minutes, then slowly decompression To 70 ~ 75 megapascal pressurize 5 minutes, it is down to 50 ~ 55 megapascal pressurize 5 minutes, is down to 15 ~ 20 megapascal pressurize 5 minutes, then is down to often Pressure;
6), open isostatic pressed cylinder cap, take out compacting tool set, carefully dismantle rubber pattern, take out the high purity niobium oxide crucible suppressed Green body;
7), crucible green body is packed into baking oven, be warming up to 100 DEG C ~ 150 DEG C, keep the temperature 24 hours, be cooled to room temperature, be packed into high temperature and burn Freezing of a furnace;
8), the crucible green body of drying is upside down in high temperature sintering furnace body, propped up with corundum tablet, prevent from deforming, be spilt on tablet Upper niobium oxide powder, haftplatte when preventing high temperature sintering;
9), high temperature sintering furnace heating process it is as follows:50 DEG C every liter keep the temperature 30 minutes, are raised to 1300 DEG C ~ 1350 DEG C always, heat preservation 2 Hour, it cools to room temperature with the furnace, comes out of the stove;
10), polishing, packaging and storage.
CN201810314735.XA 2018-04-10 2018-04-10 A kind of manufacturing method of high purity niobium oxide ontology crucible Pending CN108530066A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5940799B2 (en) * 1975-10-29 1984-10-02 住友電気工業株式会社 LINBO3 Mataha LITAO3 Notanketsushiyouno Seizouhouhou
JPS60183709A (en) * 1984-03-01 1985-09-19 Matsushita Electric Ind Co Ltd Substrate for thin film magnetic head
DE10244826B4 (en) * 2002-09-26 2012-06-28 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Arrangement for monitoring the state of wear of the refractory lining of melting furnaces, in particular glass melting tanks
CN103449845A (en) * 2013-09-11 2013-12-18 广东致远新材料有限公司 Manufacturing method of crucible for producing niobium oxide or tantalum oxide
CN104973864A (en) * 2015-07-08 2015-10-14 北京冶科纳米科技有限公司 Niobium oxide plane target preparation method and niobium oxide plane target
CN105130432A (en) * 2015-07-27 2015-12-09 江西三石有色金属有限公司 Production method of body material crucible for calcining hydroxides in tantalum and niobium smelting

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5940799B2 (en) * 1975-10-29 1984-10-02 住友電気工業株式会社 LINBO3 Mataha LITAO3 Notanketsushiyouno Seizouhouhou
JPS60183709A (en) * 1984-03-01 1985-09-19 Matsushita Electric Ind Co Ltd Substrate for thin film magnetic head
DE10244826B4 (en) * 2002-09-26 2012-06-28 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Arrangement for monitoring the state of wear of the refractory lining of melting furnaces, in particular glass melting tanks
CN103449845A (en) * 2013-09-11 2013-12-18 广东致远新材料有限公司 Manufacturing method of crucible for producing niobium oxide or tantalum oxide
CN104973864A (en) * 2015-07-08 2015-10-14 北京冶科纳米科技有限公司 Niobium oxide plane target preparation method and niobium oxide plane target
CN105130432A (en) * 2015-07-27 2015-12-09 江西三石有色金属有限公司 Production method of body material crucible for calcining hydroxides in tantalum and niobium smelting

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Application publication date: 20180914