CN107417260A - The hot pressing method for preparing of magnesia ceramics - Google Patents
The hot pressing method for preparing of magnesia ceramics Download PDFInfo
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- CN107417260A CN107417260A CN201710793212.3A CN201710793212A CN107417260A CN 107417260 A CN107417260 A CN 107417260A CN 201710793212 A CN201710793212 A CN 201710793212A CN 107417260 A CN107417260 A CN 107417260A
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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
- C04B35/01—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
- C04B35/03—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/04—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
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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
- C04B35/622—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
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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
- C04B35/622—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
- C04B35/632—Organic additives
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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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
- C04B2235/02—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
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
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- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention belongs to metallurgical technology field, and in particular to a kind of hot pressing method for preparing of magnesia ceramics.The problem of magnesia ceramics purity that is prepared for existing method is low, compactness is poor, the present invention provides a kind of hot pressing method for preparing of magnesia ceramics, comprises the following steps：A, magnesia powder is subjected to magnetic separation through electromagnetic separator, ball milling is into certain fineness after magnetic separation；B, by paraffin melting rear oxidation magnesium powder, mould is injected after well mixed；C, it is pressed using heat pressing forming machines, semi-finished product is made；D, semi-finished product are put into sintering furnace and sintered, alumina powder is blown into sintering furnace during sintering, magnesia ceramics is obtained after terminating.The inventive method is suppressed by using heat pressing forming machines, controls hot pressing condition and sintering condition so that the magnesia ceramics purity of preparation is high, compactness is high, and hardness is big.The inventive method is simple and easy, and the magnesia ceramics quality of preparation is high, has important economic benefit.
Description
Technical field
The invention belongs to metallurgical technology field, and in particular to a kind of hot pressing method for preparing of magnesia ceramics.
Background technology
Magnesia ceramics belongs to cubic system, and fusing point compares volume under 2800 DEG C or so, Mohs' hardness 5-6, high temperature
Resistance value is higher, there is good insulating properties.The high-temperature stability of magnesia ceramics, decay resistance are better than aluminium oxide ceramics, can
To be used under strong alkali corrosive atmosphere.For example made pottery applied to sodium-sulphur battery Beta aluminum oxide (β-Al2O3) solid
The high temperature sintering of porcelain electrolytic tube, alkali resistance is corroded at high temperature for it, service life length, it is normal can effectively to make up the high temperature such as corundum
Advise the deficiency that refractory material is applied in some harsh hot environments.In addition, when being contacted with many metals chemistry does not occur for magnesia
Reaction, in an inert atmosphere, even if temperature is up to 1800 DEG C, magnesia does not also react with metals such as nickel, molybdenum, niobiums.Therefore,
Magnesia tube, crucible can be used for the various steel alloys of melting, high temperature alloy without polluting alloy solution.
Magnesia ceramic articles are mostly purity or the relatively low product of consistency on domestic market, for refractory material,
Ceramic crucible and protecting tube etc..Patent 200810156563.4 discloses a kind of steel making oxygen magnesia refractories
And construction method, its product content of magnesia are 93%-95%, density<3g/cm3.Patent 201010281144.0 discloses
A kind of preparation method of high density magnesia ceramic, using nanoscale high-purity alkali type magnesium carbonate, by calcining, being molded, sintering and obtain
Magnesia ceramics is obtained, it is higher to ingredient requirement.Patent 201010563871.6 provides one kind and uses Gel-casting process system
The method of standby high density magnesia ceramic, its technique is relative complex, to use more organic matter.High purity magnesium oxide ceramics have
High temperature resistant, it is corrosion-resistant the advantages that, but the more difficult dense sintering of high purity magnesium oxide ceramics, the use of high-purity light magnesium oxide is original
Material, because its bulk density is low, reactivity is strong so that powder processed, form certain difficulty, particularly prepare the big chi of high-compactness
Phenomena such as very little magnesia tube, crucible are easily deformed, ftractureed.
The content of the invention
The technical problem to be solved in the present invention is：Magnesia ceramics purity prepared by existing method is low, compactness is poor asks
Topic.
The present invention solve technical problem technical scheme be：A kind of hot pressing method for preparing of magnesia ceramics, the party are provided
Method is simple to operate, and the magnesia ceramics purity height of preparation, compactness are good, can be widely used in the neck such as refractory material, ceramic crucible
Domain.
The invention provides a kind of hot pressing method for preparing of magnesia ceramics, comprise the following steps：
A, magnesia powder is subjected to magnetic separation through electromagnetic separator, ball milling is into certain fineness after magnetic separation；
B, added after will be paraffin melting in magnesia powder after step a ball millings, inject mould after well mixed；
C, it is pressed using heat pressing forming machines, semi-finished product is made；
D, the semi-finished product obtained by step c are put into sintering furnace and sintered, be blown alumina powder, sintering knot during sintering into sintering furnace
Magnesia ceramics is obtained after beam.
Wherein, in the hot pressing method for preparing of above-mentioned magnesia ceramics, magnetic field intensity is 0.5- during magnetic separation described in step a
2T。
Wherein, in the hot pressing method for preparing of above-mentioned magnesia ceramics, the certain fineness described in step a is 350-400 mesh.
Wherein, in the hot pressing method for preparing of above-mentioned magnesia ceramics, the paraffin that is added described in step b and magnesia powder
Weight ratio is 3-8:2-5.
Wherein, in the hot pressing method for preparing of above-mentioned magnesia ceramics, paraffin melting rear temperature is 70-90 described in step b
℃。
Wherein, in the hot pressing method for preparing of above-mentioned magnesia ceramics, the compressing condition described in step c is：Hot pressing
80-120 DEG C of temperature, hot pressing pressure 0.1-2Mpa, hot pressing time 10-30min.
Wherein, in the hot pressing method for preparing of above-mentioned magnesia ceramics, the sintering condition described in step d is：Sintering temperature
1100-1300 DEG C, sintering time 1-6h.
Wherein, in the hot pressing method for preparing of above-mentioned magnesia ceramics, described in step d be blown alumina powder purity for >=
90%, injecting velocity 0.3-0.5g/min.
Compared with prior art, beneficial effects of the present invention are：It is standby that the present invention provides a kind of hot pressing of magnesia ceramics
Method, the impurity in magnetic separation removal magnesia is first passed through, makes magnesia purity higher；Mixed again using atoleine with magnesia
Close, using the characteristic of paraffin, be easy to inject all size and the mould of shape, then suppressed using heat pressing forming machines, passed through
Control hot pressing condition and sintering condition so that the magnesia ceramics purity of preparation is high, compactness is high, and hardness is big.Present invention side
Method is simple and easy, and the magnesia ceramics quality of preparation is high, has important economic benefit.
Embodiment
The invention provides a kind of hot pressing method for preparing of magnesia ceramics, comprise the following steps：
A, by magnesia powder through electromagnetic separator carry out magnetic separation, after magnetic separation ball milling into fineness be 350-400 mesh powders；The magnetic
Magnetic field intensity is 0.5-2T when selecting；
B, added after will be paraffin melting in magnesia powder after step a ball millings, inject mould after well mixed；Paraffin and magnesia
The weight ratio of powder is 3-8:2-5；
C, it is pressed using heat pressing forming machines, semi-finished product is made；80-120 DEG C of hot pressing temperature, hot pressing pressure 0.1-
2Mpa, hot pressing time 10-30min；
D, the semi-finished product obtained by step c being put into sintering furnace and sintered, sintering temperature is 1100-1300 DEG C, sintering time 1-6h,
Alumina powder is blown during sintering into sintering furnace, magnesia ceramics is obtained after terminating；The alumina powder purity for >=
90%, injecting velocity 0.3-0.5g/min.
In the present invention, in order to reduce the impurity in magnesia, magnetic separation is first carried out using electromagnetic separator, magnetic separation can remove
The impurity such as substantial amounts of calcium, Fe, Zn, substantially can be by three oxygen in magnesia especially when magnet separator magnetic field intensity is 0.5-2T
Change two iron to remove totally, so as to reduce the influence to magnesia sintering, magnesia ceramics has higher insulating properties and high temperature resistant
Property.
Further, the present invention is by magnesia ball milling into 350-400 mesh powders, and the magnesia under this particle diameter is superfine, energy
Enough increase the density of magnesia ceramics, so as to improve the service life of magnesia ceramic articles and requirement.
The present invention is mixed after also being melted using paraffin with magnesia, and using the characteristic of paraffin, magnesium oxide powder can
It is made variously-shaped and specification, after sintering, the ceramic that density is high, hardness is big can be obtained.In order to improve magnesia ceramics
Density, be passed through the alumina powder of high-purity in sintering, magnesia semi-finished product can be protected, be notheated in sintering
Uneven and modification.
The present invention gets up above-mentioned all combinations of features, together provides a kind of hot pressing of brand-new magnesia ceramics
Preparation Method, this method can be made the magnesia ceramics that purity is higher, compactness is more preferable, hardness is bigger, improve economic benefit.
Explanation will be further explained to the embodiment of the present invention by embodiment below, but do not indicated that this
The protection domain of invention is limited in described in embodiment in scope.
Embodiment 1 prepares magnesia ceramics with the inventive method
Specific operating process is as follows：
A, by magnesia powder through electromagnetic separator carry out magnetic separation, after magnetic separation ball milling into fineness be 350 mesh powders；During the magnetic separation
Magnetic field intensity is 0.5T；
B, added after will be paraffin melting in magnesia powder after step a ball millings, inject mould after well mixed；Paraffin and magnesia
The weight ratio of powder is 3:5；
C, it is pressed using heat pressing forming machines, semi-finished product is made；80 DEG C, hot pressing pressure 0.1Mpa of hot pressing temperature, heat
The pressure time is 10min；
D, the semi-finished product obtained by step c are put into sintering furnace and sintered, sintering temperature is 1100 DEG C, sintering time 1h, during sintering
Alumina powder is blown into sintering furnace, magnesia ceramics 1 is obtained after terminating；The alumina powder purity is >=90%, injection
Speed is 0.3g/min.
Embodiment 2 prepares magnesia ceramics with the inventive method
Specific operating process is as follows：
A, by magnesia powder through electromagnetic separator carry out magnetic separation, after magnetic separation ball milling into fineness be 400 mesh powders；During the magnetic separation
Magnetic field intensity is 2T；
B, added after will be paraffin melting in magnesia powder after step a ball millings, inject mould after well mixed；Paraffin and magnesia
The weight ratio of powder is 4:1；
C, it is pressed using heat pressing forming machines, semi-finished product is made；120 DEG C, hot pressing pressure 2Mpa of hot pressing temperature, hot pressing
Time is 30min；
D, the semi-finished product obtained by step c are put into sintering furnace and sintered, sintering temperature is 1300 DEG C, sintering time 6h, during sintering
Alumina powder is blown into sintering furnace, magnesia ceramics 2 is obtained after terminating；The alumina powder purity is >=90%, injection
Speed is 0.5g/min.
Embodiment 3 prepares magnesia ceramics with the inventive method
Specific operating process is as follows：
A, by magnesia powder through electromagnetic separator carry out magnetic separation, after magnetic separation ball milling into fineness be 400 mesh powders；During the magnetic separation
Magnetic field intensity is 1T；
B, added after will be paraffin melting in magnesia powder after step a ball millings, inject mould after well mixed；Paraffin and magnesia
The weight ratio of powder is 5:3；
C, it is pressed using heat pressing forming machines, semi-finished product is made；100 DEG C, hot pressing pressure 1Mpa of hot pressing temperature, hot pressing
Time is 20min；
D, the semi-finished product obtained by step c are put into sintering furnace and sintered, sintering temperature is 1200 DEG C, sintering time 3h, during sintering
Alumina powder is blown into sintering furnace, magnesia ceramics 3 is obtained after terminating；The alumina powder purity is >=90%, injection
Speed is 0.4g/min.
Performance measurement is carried out to magnesia ceramics prepared by embodiment 1-3, obtains result of the test as shown in table 1 below.
Magnesia ceramics performance prepared by the distinct methods of table 1
From embodiment result, using the heat pressing process of the present invention, purity can be prepared higher than 98%, consistency is higher than
4.2 g/ cm3, Mohs' hardness is higher than 6 magnesia ceramics, higher, more compared to magnesia ceramics purity prepared by existing method
Densification, hardness are bigger, can increase the service life, widen using field, have obvious economic benefit.
Claims (8)
1. the hot pressing method for preparing of magnesia ceramics, it is characterised in that comprise the following steps：
A, magnesia powder is subjected to magnetic separation through electromagnetic separator, ball milling is into certain fineness after magnetic separation；
B, added after will be paraffin melting in magnesia powder after step a ball millings, inject mould after well mixed；
C, it is pressed using heat pressing forming machines, semi-finished product is made；
D, the semi-finished product obtained by step c are put into sintering furnace and sintered, be blown alumina powder, sintering knot during sintering into sintering furnace
Magnesia ceramics is obtained after beam.
2. the hot pressing method for preparing of magnesia ceramics according to claim 1, it is characterised in that：Magnetic separation described in step a
When magnetic field intensity be 0.5-2T.
3. the hot pressing method for preparing of magnesia ceramics according to claim 1, it is characterised in that：One described in step a
It is 350-400 mesh to determine fineness.
4. the hot pressing method for preparing of magnesia ceramics according to claim 1, it is characterised in that：Added described in step b
Paraffin and the weight ratio of magnesia powder be 3-8:2-5.
5. the hot pressing method for preparing of magnesia ceramics according to claim 1, it is characterised in that：Paraffin described in step b
Temperature is 70-90 DEG C after thawing.
6. the hot pressing method for preparing of magnesia ceramics according to claim 1, it is characterised in that：Pressure described in step c
Condition of molding processed is：80-120 DEG C of hot pressing temperature, hot pressing pressure 0.1-2Mpa, hot pressing time 10-30min.
7. the hot pressing method for preparing of magnesia ceramics according to claim 1, it is characterised in that：Burning described in step d
Knot condition is：1100-1300 DEG C of sintering temperature, sintering time 1-6h.
8. the hot pressing method for preparing of magnesia ceramics according to claim 1, it is characterised in that：It is blown described in step d
The purity of alumina powder is >=90%, injecting velocity 0.3-0.5g/min.
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Cited By (4)
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| CN108341659A (en) * | 2018-03-05 | 2018-07-31 | 福建省德化县驰宇陶瓷有限公司 | A kind of manufacture craft of magnesia dry-pressing ceramic products |
| CN108706966A (en) * | 2018-08-22 | 2018-10-26 | 连云港市隆泰镁业有限公司 | A kind of preparation method and application of high-purity electrically molten magnesia |
| CN110072306A (en) * | 2019-05-14 | 2019-07-30 | 安徽厘米时光电热技术有限公司 | Magnesium oxide column for electric heating tube and externally-wound electric heating tube |
| CN110087350A (en) * | 2019-05-14 | 2019-08-02 | 安徽厘米时光电热技术有限公司 | Double-end electric heating tube |
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| CN108706966A (en) * | 2018-08-22 | 2018-10-26 | 连云港市隆泰镁业有限公司 | A kind of preparation method and application of high-purity electrically molten magnesia |
| CN110072306A (en) * | 2019-05-14 | 2019-07-30 | 安徽厘米时光电热技术有限公司 | Magnesium oxide column for electric heating tube and externally-wound electric heating tube |
| CN110087350A (en) * | 2019-05-14 | 2019-08-02 | 安徽厘米时光电热技术有限公司 | Double-end electric heating tube |
| CN110087350B (en) * | 2019-05-14 | 2022-05-13 | 安徽元思电气有限公司 | Double-end electrothermal tube |
| CN110072306B (en) * | 2019-05-14 | 2022-05-13 | 安徽元思电气有限公司 | Externally-wound magnesium oxide column single-head electric heating tube |
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Application publication date: 20171201 |