CN104016669A - Magnesium ceramic crucible for sintering and preparation method thereof - Google Patents
Magnesium ceramic crucible for sintering and preparation method thereof Download PDFInfo
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- CN104016669A CN104016669A CN201410183721.0A CN201410183721A CN104016669A CN 104016669 A CN104016669 A CN 104016669A CN 201410183721 A CN201410183721 A CN 201410183721A CN 104016669 A CN104016669 A CN 104016669A
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- Prior art keywords
- sintering
- crucible
- powder
- magnesium
- magnesia
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Links
- 238000005245 sintering Methods 0.000 title claims abstract description 112
- 239000000919 ceramic Substances 0.000 title claims abstract description 27
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000011777 magnesium Substances 0.000 title claims abstract description 19
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 180
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 112
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 62
- 239000011029 spinel Substances 0.000 claims abstract description 62
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 46
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000292 calcium oxide Substances 0.000 claims abstract description 24
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 15
- 229960001866 silicon dioxide Drugs 0.000 claims abstract description 14
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims description 97
- 239000002994 raw material Substances 0.000 claims description 43
- 229910052573 porcelain Inorganic materials 0.000 claims description 40
- 235000015895 biscuits Nutrition 0.000 claims description 24
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical group [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- 238000000227 grinding Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 14
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 11
- 230000003068 static effect Effects 0.000 claims description 11
- 238000005520 cutting process Methods 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 239000012535 impurity Substances 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 7
- 239000011575 calcium Substances 0.000 abstract description 7
- 229910052791 calcium Inorganic materials 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 239000010703 silicon Substances 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 6
- 150000001340 alkali metals Chemical class 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910020068 MgAl Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 208000034809 Product contamination Diseases 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- BNOODXBBXFZASF-UHFFFAOYSA-N [Na].[S] Chemical compound [Na].[S] BNOODXBBXFZASF-UHFFFAOYSA-N 0.000 description 1
- SHPBBNULESVQRH-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].[Zr+4] Chemical compound [O-2].[O-2].[Ti+4].[Zr+4] SHPBBNULESVQRH-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a magnesium ceramic crucible for sintering and a preparation method thereof, belonging to the technical field of new material production equipment. The host crystal phase of the magnesium ceramic crucible for sintering is magnesia alumina spinel or magnesium-rich spinel; and the finished product comprises the following components in percentage by weight: 28-40% of magnesium oxide (MgO), 60-72% of aluminum oxide (Al2O3), 0-0.1% of calcium oxide (CaO) and 0-0.2% of silicon dioxide (SiO2). The magnesium ceramic crucible for sintering has low contents of impurity elements (calcium and silicon), and can avoid polluting the product. The host crystal phase of the crucible is the magnesia alumina spinel or magnesium-rich spinel, both of the two crystalline phases have alkaline atmosphere corrosion resistance, and the magnesia alumina spinel crucible is easy to sinter, is compact, and needs no or little silicon dioxide, calcium oxide and other sintering assistants.
Description
Technical field
The present invention relates to a kind of magnesia porcelain crucible and preparation method thereof, more particularly, the present invention relates to a kind of sintering magnesia porcelain crucible and preparation method thereof, belong to novel material production unit technical field.
Background technology
Pottery, owing to having good thermal conductivity, physical strength, high thermal resistance, erosion resistance, is applied more and more extensively, can be used for making high-temperature crucibles, fire-resistant boiler tube and corrosion-resistant, wear parts.Magnesia porcelain crucible use temperature taking magnesium oxide as main component is up to 1600-1850 DEG C, and chemical stability is good, and alkaline-resisting metallic vapor corrosive power is strong, is particularly suitable as crucible required in the stupalith sintering process containing lithium and sodium element or protection lining.
State Intellectual Property Office discloses a patent of invention that publication number is CN103121852A in 2013.5.29, and this patent discloses a kind of sodium-sulfur cell ionogen Na-β " Al
2o
3the magnesia crucible that ceramic post sintering is used, taking electrically molten magnesia powder, heavy-calcined magnesia powder, yttrium oxide powder, titanium dioxide zirconium powder, aluminium oxide powder, silicon-dioxide and calcium oxide powder as raw material, by being machined into again the crucible of desired size after sintering obtains blank under 1780-1860 DEG C of high temperature after isostatic pressing.The crucible of this disclosure of the invention is intended to the " Al for Na-β
2o
3in ceramic post sintering process, provide alkaline protective atmosphere suitable, suppress the quick volatilization of sodium steam in sintering process, avoid using platinum crucible as protection lining, reduce production costs.
The each material component of magnesia crucible and weight percent thereof in above-mentioned patent are as follows:
Electrically molten magnesia powder 30-80%; Heavy-calcined magnesia powder 10-40%; Yttrium oxide powder 1-10%; Zirconium dioxide powder 0.1-3%; Aluminium sesquioxide powder 0.1-3%; SiO 2 powder 0.1-3%; Lime powder 0.1-3%; The weight percent sum of all material components is 100%.
Na-β " Al
2o
3not only need material alkali resistance to corrode in the needed high-temperature heat treatment crucible of pottery of alkali metal containing element, also need to consider this oligo-element volatilizing impact on product of crucible under hot conditions.In aforementioned patent of invention, the principal crystalline phase of crucible product is magnesium oxide, and its shortcoming is:
1, the high-temperature behavior of crucible is poor, and the hot strength of crucible and wearing quality are by influenced;
2, in crucible use procedure, to the Na-β " Al of sintering in crucible
2o
3bring pollution on pottery;
If 3 solve the problems referred to above by the purity that improves raw materials of magnesium oxide, the sintering temperature of crucible is very high, need to obtain at 1800 DEG C of above long-time high temperature sinterings the crucible of certain density and intensity, causes high energy consumption.
Summary of the invention
The present invention is intended to solve the problems of the prior art, and a kind of sintering magnesia porcelain crucible and preparation method thereof is provided, and has both improved the sintering activity of crucible, and high-temperature behavior is provided, and effectively avoids introducing again contaminating impurity, and can reduce energy consumption.
To achieve these goals, the concrete technical scheme of the present invention is as follows:
A kind of sintering magnesia porcelain crucible, is characterized in that: the principal crystalline phase of described sintering magnesia porcelain crucible is magnesium-aluminium spinel or magnesium-rich spinel, in finished product, comprises following composition according to weight percent meter:
Magnesium oxide MgO 28-40%
Aluminium sesquioxide Al
2o
360-72%
Calcium oxide CaO 0-0.1%
Silicon-dioxide SiO
20-0.2%.
Total content >=99.5% of magnesium oxide of the present invention and aluminium sesquioxide.
Other impurity elements are no more than 0.5%, and especially calcium oxide impurity should be no more than 0.1%, and silicon-dioxide impurity is no more than 0.2%.
Magnesia porcelain crucible density>=3.4 g/cm of the present invention
3.
The preparation method of a kind of sintering magnesia porcelain crucible of the present invention, is characterized in that: comprise following processing step:
A, adopt magnesium oxide powder and aluminium sesquioxide powder as raw material, or adopt magnesia-alumina spinel powder as raw material, or adopt magnesium-aluminium spinel and magnesium oxide as raw material, calculate raw materials quality ratio according to crucible finished product composition quality percentage range; Wherein the median size of magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 1-100 μ m;
B, the static pressure method such as pass through after raw material is mixed and be pressed into the biscuit of required specification, pressure is 100-300MPa;
C, biscuit high temperature sintering under air atmosphere becomes ceramic blank, and sintering temperature is 1700-1800 DEG C, and sintering time is 1-5 hour;
D, ceramic blank become the crucible of desired size by cutting, ground finish;
E, crucible are incubated 1 hour in the air atmosphere of 800-1200 DEG C, and the moisture of removing grinding fluid in the course of processing and absorption obtains described sintering magnesia porcelain crucible.
The present invention is in steps A, and the median size of described magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 5-30 μ m.
The present invention is in step B, and described pressure is 150-200MPa.
The present invention is in step C, and described sintering temperature is 1750-1770 DEG C, and sintering time is 2-3 hour.
Magnesium-aluminium spinel theoretical chemistry formula of the present invention is MgOAl
2o
3, the Theoretical Mass of magnesium oxide and aluminium sesquioxide is than being 28.2:71.8.
The useful technique effect that the present invention brings:
1, the present invention finds by research, and the reason that causes background technology Patent problem is calcium and silicon, and they are to Na-β " Al
2o
3pottery conductivity and have the harmful element of material impact work-ing life, wherein introduce content is 0.1-3% separately silicon-dioxide and calcium oxide as sintering agent, under 1780-1860 DEG C of high temperature, sintering obtains crucible, it is introduced above-mentioned content sintering agent for raising sintering character and brings two drawbacks: 1, silicon oxide at high temperature has compared with high workability, so the hot strength of crucible and wearing quality are by influenced; 2, in crucible use procedure, calcium and element silicon are volatile, to the Na-β " Al of sintering in crucible
2o
3bring pollution on pottery, and be the detrimental impurity of this class pottery.And if by improving the purity of raw materials of magnesium oxide, do not introduce this class sintering aid, the sintering temperature of crucible is very high, need to obtain at 1800 DEG C of above long-time high temperature sinterings the crucible of certain density and intensity.In prior art, cannot find the reason of technical problem to be solved by this invention always, be calcium oxide and the silicon-dioxide as sintering agent and the present invention has found out its reason.
2, Na-β " Al
2o
3very responsive to the content of calcium and silicon, exceed 100ppm and will have a strong impact on product life, especially calcium, if content is too large in product, very easily cause pottery to crack in conduction sodium ion process, the calcium therefore in production process, crucible being contained and the impurity of silicon require as far as possible low, to avoid the volatilization of the impurity component in crucible polluted product under high temperature, but require highly purified especially crucible, difficulty and cost prepared by raising crucible sintering, especially domestic current industrial level.Contrast magnesia ceramics crucible of the prior art, the present invention is directed to Na-β " Al
2o
3in the needed high-temperature heat treatment crucible of pottery of alkali metal containing element, a kind of calcium is proposed, sila prime element is low, can avoid the magnesia porcelain crucible to product contamination.Crucible principal crystalline phase of the present invention is magnesium-aluminium spinel or magnesium-rich spinel, and two kinds of crystalline phases all have alkali-resistivity atmosphere corrosion ability, and the densification of magnesium-aluminium spinel crucible easy-sintering does not need or only need the seldom sintering aid such as introducing silicon-dioxide and calcium oxide of amount.Content of magnesia scope of the present invention is 28-40%, is conducive to form taking magnesium-aluminium spinel and magnesium-rich spinel as the magnesia crucible of principal crystalline phase, improves alkaline-resisting metallic element corrosive power.In addition, prior art is highly purified magnesia crucible, and sintering temperature is high (more than 1800 degree, even 1900 degree), cycle is long, and energy consumption is high, adopts specific raw material in the present invention, making finished product principal crystalline phase is magnesium-aluminium spinel or magnesium-rich spinel, the content of aluminium sesquioxide is 60-72%, can adopt lower sintering temperature (1700-1800 DEG C), and with short production cycle, energy consumption is low, can also alkali-resistivity atmosphere corrosion.
3, the present invention adopts magnesium oxide powder and aluminium sesquioxide powder as raw material, or adopt magnesia-alumina spinel powder as raw material, or adopt magnesium-aluminium spinel and magnesium oxide as raw material, calculate raw materials quality ratio according to crucible finished product composition quality percentage range; Wherein the median size of magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 1-100 μ m, and within the scope of this, the powder sintering activity of particle diameter is good, easily sintered ceramic.Further, the median size of described magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is preferably 5-30 μ m, this particle size range the best, and in this particle size range, powder is existing good sintering activity, the powder of easily preparing again.
4, the present invention the static pressure method such as passes through and is pressed into the biscuit of required specification after raw material is mixed, pressure is 100-300MPa, can obtain the biscuit of some strength and density in this pressure range, non-friable in the demoulding and operating process, the too small biscuit insufficient strength of pressure, the excessive demoulding of pressure is not easy.Further, pressure is preferably 150-200MPa, and biscuit intensity and the easy degree of the demoulding of compacting are all the most desirable.
5, crucible of the present invention is incubated 1 hour in the air atmosphere of 800-1200 DEG C, and the moisture of removing grinding fluid in the course of processing and absorption obtains described sintering magnesia porcelain crucible.Magnesia porcelain is the easy moisture absorption the material with water deferred reaction, and removing crystal water need to be in the above temperature of 800 degree, and 1200 degree are more reasonable for the upper limit, are incubated and within 1 hour, can ensure that crystal water removes substantially, and can keep lower energy consumption.
6, the present invention is in step C, and further sintering temperature is preferably 1750-1770 DEG C, and sintering time is 2-3 hour.Ceramic dense degree and intensity that this temperature range is fired are the most desirable.
Embodiment
embodiment 1:
The powder that adopts following feature is as raw material:
Chemical formula is MgAl
2o
4; Crystalline phase is magnesium-aluminium spinel, and powder purity is not less than 99%, CaO, SiO
2content of impurities is no more than 0.2%, powder median size 10-20 μ m.
Material powder, by waiting static pressure method pressurize 5 minutes under 180MPa, is pressed into an end opening, the flat sealing in one end, external diameter 120mm, the crucible shape biscuit of wall thickness 6mm.
Biscuit high temperature sintering under air atmosphere becomes ceramic blank, and sintering temperature is 1720 DEG C, and sintering time is 2 hours.
Ceramic blank carries out refine by cutting and method for grinding.
Crucible is incubated one hour in 1000 DEG C of left and right air atmospheres, removes the grinding fluid in the course of processing, obtains dry pure magnesium-aluminium spinel crucible, can be used for sintering Na-β " Al
2o
3deng pottery and the powder of alkali metal containing element.
embodiment 2
Magnesia powder, aluminum oxide powder are mixed according to following proportioning:
MgO：28.2%；
Al
2O
3：71.8%；
Wherein MgO, Al
2o
3purity is not less than 99%, CaO, SiO
2content of impurities is no more than 0.2%; ; Magnesium oxide powder median size 10 μ m left and right, alumina powder jointed median size is 10 μ m left and right.
After mixing, raw material by waiting static pressure method pressurize 2 minutes under 150MPa, is pressed into both ends open, external diameter 120mm, wall thickness 6mm, the biscuit pipe of long 200mm left and right.
Biscuit high temperature sintering under air atmosphere becomes ceramic blank, and sintering temperature is 1780 DEG C, and sintering time is 2 hours.
Ceramic blank carries out refine by cutting and method for grinding.
Crucible is incubated one hour in 1000 DEG C of left and right air atmospheres, removes the grinding fluid in the course of processing, obtains dry pure tubulose magnesium-aluminium spinel crucible, can be used for sintering Na-β " Al
2o
3deng the vitrified pipe of alkali metal containing element.
embodiment 3
Magnesium aluminium spinel powder, aluminum oxide powder are mixed according to following proportioning:
MgAl
20
4：85%；
MgO：15%；
Wherein MgO, MgAl
20
4purity is not less than 99%, CaO, SiO
2content of impurities is no more than 0.3%; ; Magnesium oxide powder median size 10 μ m left and right, magnesia-alumina spinel powder median size is 10 μ m left and right.
After mixing, raw material by waiting static pressure method pressurize 1 minute under 200MPa, is pressed into an end opening, 10mm left and right aperture is opened at the flat center of the other end, external diameter 100mm, wall thickness 5mm, the biscuit pipe of long 400mm.
Biscuit high temperature sintering under air atmosphere becomes ceramic blank, and sintering temperature is 1760 DEG C, and sintering time is 2 hours.
Vitrified pipe carries out refine by cutting and external grinding.
Crucible is incubated one hour in 1000 DEG C of left and right air atmospheres, removes the grinding fluid in the course of processing, obtains dry pure tubulose magnesium-rich spinel crucible, can be used for sintering Na-β " Al
2o
3deng the vitrified pipe of alkali metal containing element.
embodiment 4
Magnesia powder, aluminum oxide powder, yttrium oxide powder are mixed according to following proportioning:
MgO：35%；
Al
2O
3：65%；
Wherein MgO, Al
2o
3purity is not less than 99%, CaO, SiO
2content of impurities is no more than 0.3%; ; Magnesium oxide powder median size 20 μ m left and right, alumina powder jointed median size is 20 μ m left and right.
After mixing, raw material by waiting static pressure method pressurize 1 minute under 250MPa, is pressed into both ends open, external diameter 150mm, wall thickness 8mm, the biscuit pipe of long 300mm.
Biscuit high temperature sintering under air atmosphere becomes ceramic blank, and sintering temperature is 1800 DEG C, and sintering time is 3 hours.
Vitrified pipe carries out refine by cutting and external grinding.
Crucible is incubated one hour in 1000 DEG C of left and right air atmospheres, removes the grinding fluid in the course of processing, obtains dry pure tubulose magnesium-rich spinel crucible, can be used for sintering Na-β " Al
2o
3deng the vitrified pipe of alkali metal containing element.
embodiment 5
A kind of sintering magnesia porcelain crucible, the principal crystalline phase of described sintering magnesia porcelain crucible is magnesium-aluminium spinel or magnesium-rich spinel, in finished product, comprises following composition according to weight percent meter:
Magnesium oxide MgO 28%
Aluminium sesquioxide Al
2o
372%
Calcium oxide CaO 0%
Silicon-dioxide SiO
20%.
embodiment 6
A kind of sintering magnesia porcelain crucible, the principal crystalline phase of described sintering magnesia porcelain crucible is magnesium-aluminium spinel or magnesium-rich spinel, in finished product, comprises following composition according to weight percent meter:
Magnesium oxide MgO 40%
Aluminium sesquioxide Al
2o
360%
Calcium oxide CaO 0%
Silicon-dioxide SiO
20%.
embodiment 7
A kind of sintering magnesia porcelain crucible, the principal crystalline phase of described sintering magnesia porcelain crucible is magnesium-aluminium spinel or magnesium-rich spinel, in finished product, comprises following composition according to weight percent meter:
Magnesium oxide MgO 33.9%
Aluminium sesquioxide Al
2o
365.8%
Calcium oxide CaO 0.1%
Silicon-dioxide SiO
20.2%.
embodiment 8
A kind of sintering magnesia porcelain crucible, the principal crystalline phase of described sintering magnesia porcelain crucible is magnesium-aluminium spinel or magnesium-rich spinel, in finished product, comprises following composition according to weight percent meter:
Magnesium oxide MgO 29.7%
Aluminium sesquioxide Al
2o
370.2%
Calcium oxide CaO 0-%
Silicon-dioxide SiO
20.1%.
embodiment 9
A kind of sintering magnesia porcelain crucible, the principal crystalline phase of described sintering magnesia porcelain crucible is magnesium-aluminium spinel or magnesium-rich spinel, in finished product, comprises following composition according to weight percent meter:
Magnesium oxide MgO 38.6%
Aluminium sesquioxide Al
2o
361.35%
Calcium oxide CaO 0.05%
Silicon-dioxide SiO
20%.
embodiment 10
The preparation method of crucible:
The preparation method of a kind of sintering magnesia porcelain crucible of the present invention, is characterized in that: comprise following processing step:
A, adopt magnesium oxide powder and aluminium sesquioxide powder as raw material, or adopt magnesia-alumina spinel powder as raw material, or adopt magnesium-aluminium spinel and magnesium oxide as raw material, calculate raw materials quality ratio according to crucible finished product composition quality percentage range; Wherein the median size of magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 1 μ m;
B, the static pressure method such as pass through after raw material is mixed and be pressed into the biscuit of required specification, pressure is 100MPa;
C, biscuit high temperature sintering under air atmosphere becomes ceramic blank, and sintering temperature is 1700 DEG C, and sintering time is 1 hour;
D, ceramic blank become the crucible of desired size by cutting, ground finish;
E, crucible are incubated 1 hour in the air atmosphere of 800 DEG C, and the moisture of removing grinding fluid in the course of processing and absorption obtains described sintering magnesia porcelain crucible.
Further preferred:
The present invention is in steps A, and the median size of described magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 5 μ m.
The present invention is in step B, and described pressure is 150MPa.
The present invention is in step C, and described sintering temperature is 1750 DEG C, and sintering time is 2 hours.
embodiment 11
The preparation method of crucible:
The preparation method of a kind of sintering magnesia porcelain crucible of the present invention, is characterized in that: comprise following processing step:
A, adopt magnesium oxide powder and aluminium sesquioxide powder as raw material, or adopt magnesia-alumina spinel powder as raw material, or adopt magnesium-aluminium spinel and magnesium oxide as raw material, calculate raw materials quality ratio according to crucible finished product composition quality percentage range; Wherein the median size of magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 100 μ m;
B, the static pressure method such as pass through after raw material is mixed and be pressed into the biscuit of required specification, pressure is 300MPa;
C, biscuit high temperature sintering under air atmosphere becomes ceramic blank, and sintering temperature is 1800 DEG C, and sintering time is 5 hours;
D, ceramic blank become the crucible of desired size by cutting, ground finish;
E, crucible are incubated 1 hour in the air atmosphere of 1200 DEG C, and the moisture of removing grinding fluid in the course of processing and absorption obtains described sintering magnesia porcelain crucible.
Further preferred:
The present invention is in steps A, and the median size of described magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 30 μ m.
The present invention is in step B, and described pressure is 200MPa.
The present invention is in step C, and described sintering temperature is 1770 DEG C, and sintering time is 3 hours.
embodiment 12
The preparation method of crucible:
The preparation method of a kind of sintering magnesia porcelain crucible of the present invention, is characterized in that: comprise following processing step:
A, adopt magnesium oxide powder and aluminium sesquioxide powder as raw material, or adopt magnesia-alumina spinel powder as raw material, or adopt magnesium-aluminium spinel and magnesium oxide as raw material, calculate raw materials quality ratio according to crucible finished product composition quality percentage range; Wherein the median size of magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 50 μ m;
B, the static pressure method such as pass through after raw material is mixed and be pressed into the biscuit of required specification, pressure is 200MPa;
C, biscuit high temperature sintering under air atmosphere becomes ceramic blank, and sintering temperature is 1750 DEG C, and sintering time is 3 hours;
D, ceramic blank become the crucible of desired size by cutting, ground finish;
E, crucible are incubated 1 hour in the air atmosphere of 1000 DEG C, and the moisture of removing grinding fluid in the course of processing and absorption obtains described sintering magnesia porcelain crucible.
Further preferred:
The present invention is in steps A, and the median size of described magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 18 μ m.
The present invention is in step B, and described pressure is 175MPa.
The present invention is in step C, and described sintering temperature is 1760 DEG C, and sintering time is 2.5 hours.
embodiment 13
The preparation method of crucible:
The preparation method of a kind of sintering magnesia porcelain crucible of the present invention, is characterized in that: comprise following processing step:
A, adopt magnesium oxide powder and aluminium sesquioxide powder as raw material, or adopt magnesia-alumina spinel powder as raw material, or adopt magnesium-aluminium spinel and magnesium oxide as raw material, calculate raw materials quality ratio according to crucible finished product composition quality percentage range; Wherein the median size of magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 80 μ m;
B, the static pressure method such as pass through after raw material is mixed and be pressed into the biscuit of required specification, pressure is 120MPa;
C, biscuit high temperature sintering under air atmosphere becomes ceramic blank, and sintering temperature is 1720 DEG C, and sintering time is 4.5 hours;
D, ceramic blank become the crucible of desired size by cutting, ground finish;
E, crucible are incubated 1 hour in the air atmosphere of 1100 DEG C, and the moisture of removing grinding fluid in the course of processing and absorption obtains described sintering magnesia porcelain crucible.
Further preferred:
The present invention is in steps A, and the median size of described magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 7 μ m.
The present invention is in step B, and described pressure is 160MPa.
The present invention is in step C, and described sintering temperature is 1766 DEG C, and sintering time is 2.25 hours.
Claims (6)
1. a sintering magnesia porcelain crucible, is characterized in that: the principal crystalline phase of described sintering magnesia porcelain crucible is magnesium-aluminium spinel or magnesium-rich spinel, in finished product, comprises following composition according to weight percent meter:
Magnesium oxide MgO 28-40%
Aluminium sesquioxide Al
2o
360-72%
Calcium oxide CaO 0-0.1%
Silicon-dioxide SiO
20-0.2%.
2. a kind of sintering magnesia porcelain crucible according to claim 1, is characterized in that: described magnesia porcelain crucible density>=3.4 g/cm
3.
3. the preparation method of a kind of sintering magnesia porcelain crucible according to claim 1 and 2, is characterized in that: comprise following processing step:
A, adopt magnesium oxide powder and aluminium sesquioxide powder as raw material, or adopt magnesia-alumina spinel powder as raw material, or adopt magnesium-aluminium spinel and magnesium oxide as raw material, calculate raw materials quality ratio according to crucible finished product composition quality percentage range; Wherein the median size of magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 1-100 μ m;
B, the static pressure method such as pass through after raw material is mixed and be pressed into the biscuit of required specification, pressure is 100-300MPa;
C, biscuit high temperature sintering under air atmosphere becomes ceramic blank, and sintering temperature is 1700-1800 DEG C, and sintering time is 1-5 hour;
D, ceramic blank become the crucible of desired size by cutting, ground finish;
E, crucible are incubated 1 hour in the air atmosphere of 800-1200 DEG C, and the moisture of removing grinding fluid in the course of processing and absorption obtains described sintering magnesia porcelain crucible.
4. the preparation method of a kind of sintering magnesia porcelain crucible according to claim 3, is characterized in that: in steps A, the median size of described magnesium oxide powder, magnesia-alumina spinel powder and aluminium sesquioxide powder is 5-30 μ m.
5. the preparation method of a kind of sintering magnesia porcelain crucible according to claim 3, is characterized in that: in step B, described pressure is 150-200MPa.
6. the preparation method of a kind of sintering magnesia porcelain crucible according to claim 3, is characterized in that: in step C, described sintering temperature is 1750-1770 DEG C, and sintering time is 2-3 hour.
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| CN105837181A (en) * | 2016-03-28 | 2016-08-10 | 上海电气钠硫储能技术有限公司 | Crucible for synthesis of [beta]''-aluminum oxide powder and production method thereof |
| CN107417260A (en) * | 2017-09-06 | 2017-12-01 | 盐城市华康电热绝缘材料厂 | The hot pressing method for preparing of magnesia ceramics |
| CN108546091A (en) * | 2018-05-09 | 2018-09-18 | 肃北镁弘科技有限公司 | A kind of preparation method of surface coated magnesia crucible |
| CN110762012A (en) * | 2019-11-08 | 2020-02-07 | 广东美芝精密制造有限公司 | Compressor, refrigeration equipment and preparation method of middle partition plate |
| CN111393169A (en) * | 2020-03-27 | 2020-07-10 | 山东铭特陶瓷材料有限公司 | Magnesium aluminate spinel crucible for high-temperature alloy and preparation method thereof |
| CN112321282A (en) * | 2020-11-05 | 2021-02-05 | 山东瑞泰新材料科技有限公司 | High-strength magnesium oxide crucible and preparation method thereof |
| CN113814360A (en) * | 2021-09-18 | 2021-12-21 | 江西理工大学 | Rare earth steel spectrum standard sample and preparation method thereof |
| CN115231916A (en) * | 2022-07-13 | 2022-10-25 | 西安西工大思强科技股份有限公司 | Magnesium aluminate spinel forming crucible and manufacturing method thereof |
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| CN105837181A (en) * | 2016-03-28 | 2016-08-10 | 上海电气钠硫储能技术有限公司 | Crucible for synthesis of [beta]''-aluminum oxide powder and production method thereof |
| CN107417260A (en) * | 2017-09-06 | 2017-12-01 | 盐城市华康电热绝缘材料厂 | The hot pressing method for preparing of magnesia ceramics |
| CN108546091A (en) * | 2018-05-09 | 2018-09-18 | 肃北镁弘科技有限公司 | A kind of preparation method of surface coated magnesia crucible |
| CN110762012A (en) * | 2019-11-08 | 2020-02-07 | 广东美芝精密制造有限公司 | Compressor, refrigeration equipment and preparation method of middle partition plate |
| CN111393169A (en) * | 2020-03-27 | 2020-07-10 | 山东铭特陶瓷材料有限公司 | Magnesium aluminate spinel crucible for high-temperature alloy and preparation method thereof |
| CN112321282A (en) * | 2020-11-05 | 2021-02-05 | 山东瑞泰新材料科技有限公司 | High-strength magnesium oxide crucible and preparation method thereof |
| CN113814360A (en) * | 2021-09-18 | 2021-12-21 | 江西理工大学 | Rare earth steel spectrum standard sample and preparation method thereof |
| CN113814360B (en) * | 2021-09-18 | 2023-08-11 | 江西理工大学 | Rare earth steel spectrum standard sample and preparation method thereof |
| CN115231916A (en) * | 2022-07-13 | 2022-10-25 | 西安西工大思强科技股份有限公司 | Magnesium aluminate spinel forming crucible and manufacturing method thereof |
| CN115231916B (en) * | 2022-07-13 | 2023-08-15 | 西安西工大思强科技股份有限公司 | Magnesia-alumina spinel forming crucible and manufacturing method thereof |
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