CN108358631A - A kind of manufacturing method of high purity tantalum oxide ontology crucible - Google Patents
A kind of manufacturing method of high purity tantalum oxide ontology crucible Download PDFInfo
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- CN108358631A CN108358631A CN201810105276.4A CN201810105276A CN108358631A CN 108358631 A CN108358631 A CN 108358631A CN 201810105276 A CN201810105276 A CN 201810105276A CN 108358631 A CN108358631 A CN 108358631A
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- C—CHEMISTRY; METALLURGY
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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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/495—Shaped 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
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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
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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Abstract
A kind of manufacturing method of high purity tantalum oxide ontology crucible, the technical solution of the manufacturing method are：High purity tantalum oxide powder is by dispensing, granulation, compacting, drying, high temperature sintering, annealing, polishing, finished product.This method has the advantages that rational technology, manufacturing cost are low, and 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
Technical field
The present invention relates to a kind of manufacturing methods of high purity tantalum oxide ontology crucible.
Background technology
At present the production method of tantalum 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 tantalum oxide ontology crucible, solves high pure zirconia
The manufacturing issue of tantalum this system crucible, this method rational technology, manufacturing cost are low, and 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.
It adopts the technical scheme that, a kind of manufacturing method of high purity tantalum oxide ontology crucible, wraps to achieve the above object
Include following steps：
1), high purity tantalum oxide powder is allocated, amount of preparation 100kg meters, wherein：60% ~ 70% high purity tantalum oxide, 20% ~ 25%
Ultra-pure water, 10% ~ 15% bonding agent, the bonding agent PVA contents 5% ~ 10% add 100mL ~ 300mL dispersants, the dispersion
Agent is A135, is put into 300L wet milks；
2) 30 kg of tantalum alloy ball ~ 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 tantalum oxide particle；
4) 1.7kg ~ 1.9kg granulation high purity tantalum oxides, are taken to be fitted into rubber mold, rubber die locking prevents leak；
5) mold that, will feed is put into isostatic pressed cylinder body, slowly boosts 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) isostatic pressed cylinder cap, is opened, compacting tool set is taken out, carefully dismantles rubber pattern, take out the high purity tantalum oxide crucible suppressed
Green body；
7) crucible green body, is packed into baking oven, is warming up to 100 DEG C ~ 150 DEG C, 24 hours is kept the temperature, is cooled to room temperature, high temperature is packed into and burns
Freezing of a furnace；
8), the crucible green body of drying is upside down in high temperature sintering furnace body, is propped up with corundum tablet, prevents from deforming, be spilt on tablet
Upper oxidation tantalum powder, haftplatte when preventing high temperature sintering；
9) it is as follows, to carry out high temperature sintering furnace heating process：50 DEG C every liter keep the temperature 30 minutes, are raised to 1450 DEG C ~ 1550 DEG C always, protect
Temperature 2 hours, cools to room temperature with the furnace, comes out of the stove；
10) it, polishes, packaging and storage.
Advantageous effect
The present invention has the following advantages compared with prior art.
It is an advantage of the invention that solving the manufacturing issue of high purity tantalum oxide this system crucible, there is rational technology, manufacture
It is at low cost, 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, use
Period is long, durability is high.
Specific implementation mode
A kind of manufacturing method of high purity tantalum oxide ontology crucible, includes the following steps：
1), high purity tantalum oxide powder is allocated, amount of preparation 100kg meters, wherein：60% ~ 70% high purity tantalum oxide, 20% ~ 25%
Ultra-pure water, 10% ~ 15% bonding agent, the bonding agent PVA contents 5% ~ 10% add 100mL ~ 300mL dispersants, the dispersion
Agent is A135, is put into 300L wet milks；
2) 30 kg of tantalum alloy ball ~ 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 tantalum oxide particle；
4) 1.7kg ~ 1.9kg granulation high purity tantalum oxides, are taken to be fitted into rubber mold, rubber die locking prevents leak；
5) mold that, will feed is put into isostatic pressed cylinder body, slowly boosts 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) isostatic pressed cylinder cap, is opened, compacting tool set is taken out, carefully dismantles rubber pattern, take out the high purity tantalum oxide crucible suppressed
Green body；
7) crucible green body, is packed into baking oven, is warming up to 100 DEG C ~ 150 DEG C, 24 hours is kept the temperature, is cooled to room temperature, high temperature is packed into and burns
Freezing of a furnace；
8), the crucible green body of drying is upside down in high temperature sintering furnace body, is propped up with corundum tablet, prevents from deforming, be spilt on tablet
Upper oxidation tantalum powder, haftplatte when preventing high temperature sintering；
9) it is as follows, to carry out high temperature sintering furnace heating process：50 DEG C every liter keep the temperature 30 minutes, are raised to 1450 DEG C ~ 1550 DEG C always, protect
Temperature 2 hours, cools to room temperature with the furnace, comes out of the stove；
10) it, polishes, packaging and storage.
Embodiment one
1, high purity tantalum oxide powder is allocated, 65% high purity tantalum oxide, 23% ultra-pure water, 12% bonding agent（PVA contents 5%）,
Add 300mL dispersants（A135）Solution is put into 300L wet milks；
2,40 kilograms of tantalum alloy ball is added；
3, powders mixture ball milling 2 hours, after taking sizing liquor to cross 800 mesh sieve, spray drying obtains mobility and is less than 120 seconds
Nearly ball-type high purity tantalum oxide particle；
4,1.75kg granulation high purity tantalum 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 17 megapascal pressurize 5 minutes, then be down to normal pressure；
6, isostatic pressed cylinder cap is opened, mold is taken out, carefully 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, prevented from deforming, be sprinkled on tablet
Tantalum powder is aoxidized, 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 1480 DEG C always, 2 hours are kept the temperature, with stove
It is cooled to room temperature；
10, it polishes, packaging and storage.
One gained high purity tantalum 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：14.1Mpa；
Deformation rate：Less than 1%；
Heat rate：More than 1000 times.
Embodiment two
1, high purity tantalum oxide powder is allocated, 67% high purity niobium oxide, 23% ultra-pure water, 11% bonding agent（PVA contents 5%）,
Add 250mL dispersants（A135）Solution is put into 300L wet milks；
2, tantalum alloy ball 40kg is added；
3, powders mixture ball milling 2 hours, after taking slurries to cross 500 mesh sieve, it is close less than 100 seconds to obtain mobility for spray drying
Ball-type high purity tantalum oxide particle；
4,1.85kg high purity tantalum 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, carefully 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, protect 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
Tantalum 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 1520 DEG C always, 2 hours are kept the temperature, with stove
It is cooled to room temperature,
10, it polishes, packaging and storage.
Two gained high purity tantalum 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：15.1Mpa；
Deformation rate：Less than 1%；
Heat rate：More than 1000 times.
Claims (1)
1. a kind of manufacturing method of high purity tantalum oxide ontology crucible, which is characterized in that include the following steps：
1), high purity tantalum oxide powder is allocated, amount of preparation 100kg meters, wherein：60% ~ 70% high purity tantalum oxide, 20% ~ 25%
Ultra-pure water, 10% ~ 15% bonding agent, the bonding agent PVA contents 5% ~ 10% add 100mL ~ 300mL dispersants, the dispersion
Agent is A135, is put into 300L wet milks；
2) 30 kg of tantalum alloy ball ~ 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 tantalum oxide particle；
4) 1.7kg ~ 1.9kg granulation high purity tantalum oxides, are taken to be fitted into rubber mold, rubber die locking prevents leak；
5) mold that, will feed is put into isostatic pressed cylinder body, slowly boosts 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) isostatic pressed cylinder cap, is opened, compacting tool set is taken out, carefully dismantles rubber pattern, take out the high purity tantalum oxide crucible suppressed
Green body；
7) crucible green body, is packed into baking oven, is warming up to 100 DEG C ~ 150 DEG C, 24 hours is kept the temperature, is cooled to room temperature, high temperature is packed into and burns
Freezing of a furnace；
8), the crucible green body of drying is upside down in high temperature sintering furnace body, is propped up with corundum tablet, prevents from deforming, be spilt on tablet
Upper oxidation tantalum powder, haftplatte when preventing high temperature sintering；
9) it is as follows, to carry out high temperature sintering furnace heating process：50 DEG C every liter keep the temperature 30 minutes, are raised to 1450 DEG C ~ 1550 DEG C always, protect
Temperature 2 hours, cools to room temperature with the furnace, comes out of the stove；
10) it, polishes, packaging and storage.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810105276.4A CN108358631A (en) | 2018-02-02 | 2018-02-02 | A kind of manufacturing method of high purity tantalum oxide ontology crucible |
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| CN201810105276.4A CN108358631A (en) | 2018-02-02 | 2018-02-02 | A kind of manufacturing method of high purity tantalum oxide ontology crucible |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3969123A (en) * | 1975-02-11 | 1976-07-13 | The United States Of America As Represented By The United States Energy Research And Development Administration | Refractory ceramic compositions and method for preparing same |
| CN101318818A (en) * | 2008-07-22 | 2008-12-10 | 景德镇市科宏特种陶瓷有限公司 | Process for manufacturing high-purity niobium oxide, tantalum oxide ceramic crucible pot and manufactured products thereof |
| 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 |
-
2018
- 2018-02-02 CN CN201810105276.4A patent/CN108358631A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3969123A (en) * | 1975-02-11 | 1976-07-13 | The United States Of America As Represented By The United States Energy Research And Development Administration | Refractory ceramic compositions and method for preparing same |
| CN101318818A (en) * | 2008-07-22 | 2008-12-10 | 景德镇市科宏特种陶瓷有限公司 | Process for manufacturing high-purity niobium oxide, tantalum oxide ceramic crucible pot and manufactured products thereof |
| 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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