CN1310325A - Magnesia crucible with calcium oxide coating and its making process - Google Patents
Magnesia crucible with calcium oxide coating and its making process Download PDFInfo
- Publication number
- CN1310325A CN1310325A CN 00110150 CN00110150A CN1310325A CN 1310325 A CN1310325 A CN 1310325A CN 00110150 CN00110150 CN 00110150 CN 00110150 A CN00110150 A CN 00110150A CN 1310325 A CN1310325 A CN 1310325A
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- China
- Prior art keywords
- coating
- crucible
- cao
- temperature
- calcium oxide
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- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000000292 calcium oxide Substances 0.000 title claims abstract description 38
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 15
- 239000011248 coating agent Substances 0.000 title claims description 30
- 238000000576 coating method Methods 0.000 title claims description 30
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 title claims description 12
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 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 8
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 7
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000001110 calcium chloride Substances 0.000 claims abstract description 6
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 6
- 235000012255 calcium oxide Nutrition 0.000 claims description 35
- 238000001035 drying Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 230000036571 hydration Effects 0.000 claims description 2
- 238000006703 hydration reaction Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 235000011148 calcium chloride Nutrition 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 abstract 1
- 229910045601 alloy Inorganic materials 0.000 description 16
- 239000000956 alloy Substances 0.000 description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 238000003723 Smelting Methods 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910000640 Fe alloy Inorganic materials 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052774 Proactinium Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Crucibles And Fluidized-Bed Furnaces (AREA)
Abstract
The magnesia crucible with one 5-20 mm thick CaO layer on its inner wall is made through mixing homogeneously analytically pure CaO, Al2O3, CaCl2 and C2H5OH in the weight ratio of 100 to 0.8-1.2 to 0.4-0.6 to 53-57 and pressing the mixture together with crucible base. The present invention has low cost and simple process.
Description
The invention relates to a smelting technology of high-temperature alloy, and particularly provides a preparation method of a magnesium oxide crucible with a calcium oxide coating, which is used for smelting Ni-based high-temperature alloy.
Years of research shows that the performance of the high-temperature alloy is better than the content of impurities such as sulfur, phosphorus, nitrogen, oxygen and the like in the alloy, the strict control of the content of the impurities in the smelting process of the high-temperature alloy has important significance, the aim of achieving the aim by only selecting raw materials is obviously insufficient, the research shows that the selection of a crucible in the smelting process is also an important link, and the pure CaO crucible is considered as the first choice for smelting the high-temperature alloy at present. Such as "calcium oxide" in the literatureApplication of crucible in high purity alloy purification research, volume 34, P731-7343 of No. 7 of "journal of metals" 1998.7, Sun Changjie et al, studied purification process of melting metals and alloys in vacuum induction furnace using calcium oxide crucible. A calcium oxide crucible with good refining and heat preservation performance is manufactured by adopting a furnace knotting induction sintering method and vacuum induction at 10kg, and purification tests are carried out on pure iron and GH169 alloy by adding Al, La and Ca. The result shows that the calcium oxide crucible is used for refining at 1400 ℃ under the vacuum degree of 1.5-2.5 Pa, Al and La are added as purifying agents, the O, N content is reduced to below 20ppm after refining for 45min, and the S content is reduced to below 3 ppm. The mechanism by which the calcium oxide crucible participates in the removal of O, N and S from the alloy is also discussed. In the document "adding Al and Al alloy to CaO crucible to cause the de-S behavior of molten iron" [ iron and Steel No. 1987.14P 1684 to 16903, Chuantong et Al, for the purpose of carrying out de-O and de-S studies on iron and iron alloy, there is also provided a method for manufacturing CaO crucible, which comprises pulverizing special grade CaO reagent to 20mush, and mixing with CaCl as binder2+C2H5OH is mixed and compacted into an integral CaO crucible with the inner diameter phi of 50mm, the outer diameter phi of 70mm and the height of 160 mm. The above integrally produced CaO crucible; obviously, the cost is high and the process is complex. In the document "removing O and S from iron and iron alloy liquid by Ca and Al using CaO crucible" [ iron and Steel No. 1975.9P 19-33,2167-21811, Muuguepin et Al, there is provided a method for manufacturing a crucible for removing O and S in the melting of iron and iron alloy, comprising the steps of crushing a primary reagent CaO into 20mush, preparing a coating material by using 5% acetic acid and methanol as binders, and coating the coating material on an outer layer Al2O3The method for coating the CaO coating in the alumina crucible has the advantages of obviously low density and large porosity, is only suitable for experimental study and is not suitable for actual production.
The invention aims to provide a magnesium oxide crucible with a calcium oxide coating and a preparation method thereof, which have low cost and simple method.
The invention provides a magnesium oxide crucible with a calcium oxide coating, which is characterized in that: a layer of CaO is pressed on the inner wall of the MgO crucible, and the thickness is 5-20 mm.
The invention also provides a preparation method of the magnesium oxide crucible with the calcium oxide coating, which is characterized by comprising the following steps: selecting analytically pure CaO and Al2O3、CaCl2、C2H5OH is uniformly mixed according to the weight ratio of 100: 0.8-1.2: 0.4-0.6: 53-57, and the mixture is compacted with a crucible on a press machine to form a CaO coating, wherein the parameters are as follows:
density of wet mixture: 1.60-1.66 g/cm3
Density after hydration: 2.6 to 3.0g/cm3
Density of the coating: o-3.2 g/cm3
Porosity: 25 to 30 percent
After the coating is pressed, the coating is put into a dryer for natural drying for 46 to 52 hours, and then the coating is dried according to the following process: at room temperature Keeping the temperature for 1 to 2 hours at the temperature of between 100 and 120 DEG C Keeping the temperature for 2 to 3 hours at the temperature of between 600 and 640 DEG C Keeping the temperature at 1000-1100 ℃ for 2-3 hours, cooling the mixture to 140-160 ℃ along with the furnace, and putting the mixture into a dryer for storage for later use.
The invention presses a CaO coating in the MgO crucible, and the CaO coating is used with the MgO crucible after sintering, thus compared with the integral manufacture of the CaO crucible, the invention can reduce the cost of the crucible and simplify the production process. Compared with the process method disclosed by the literature, the density of the coating is improved, and the porosity is reduced, so that the coating can be used for actual production. The crucible is used for smelting Ni-based high-temperature alloy for the first time, and trace impurity elements in the high-temperature alloy can be well removed. The CaO coated crucible pressed by the method is used for smelting Ni-based high-temperature alloy, the N content in the Ni-based high-temperature alloy can be obviously reduced, the N content of the Ni-based high-temperature alloy with the same mark smelted by the MgO crucible is 8-26 ppm, and the N content is 1-4 ppm by adopting the CaO coated crucible.
Example 1.
CaO:750g、CaCl2:3.75g、Al2O3:7.5g、C2H5312.5g of OH is uniformly mixed and then is compacted into a coating with the thickness of 10mm in a 10kg MgO crucible, and after the coating is treated and dried by the process, the Ni-based high-temperature alloy is smelted on a 25kg vacuum casting furnace, thereby obtaining better results. The N removing effect is as follows:
| heat of furnace | 1 | 2 | 3 | 4 |
| Content of N (ppm) | 5 | 3 | 3 | 2 |
Example 2.
CaO:750g、CaCl2:3.5g、Al2O3:7g、C2H5OH 315g other procedures were as above. The N removing effect is as follows:
| heat of furnace | 1 | 2 | 3 | 4 |
| Content of N (ppm) | 4 | 3 | 3 | 3 |
Example 3.
CaO:750g、CaCl2:3.6g、Al2O3:8g、C2H5OH 318g other procedures were as above. The N removing effect is as follows:
| heat of furnace | 1 | 2 | 3 | 4 |
| Content of N (ppm) | 3 | 2 | 1 | 2 |
Comparative example
Similarly, if the above proportioning is not performed according to the drying process, for example, the following process is performed: at room temperature Keeping the temperature for 0.5 hour at 100-120 DEG C Keeping the temperature for 1 hour at 600-620 DEG C 1000-1100 deg.C, heat-insulating for 1 hr → placing in a drier for storage when the furnace is cooled to 150 deg.C, the coating will be peeled off and cracked, and can not be used.
Claims (2)
1. A magnesia crucible with a calcium oxide coating is characterized in that: a layer of CaO is pressed on the inner wall of the MgO crucible, and the thickness is 5-20 mm.
2. A method for preparing a magnesia crucible having a calcia coating according to claim 1, characterized in that: selecting analytically pure CaO and Al2O3、CaCl2、C2H5OH is uniformly mixed according to the weight ratio of 100: 0.8-1.2: 0.4-0.6: 53-57, and the mixture is compacted with a crucible on a press machine to form a CaO coating, wherein the parameters are as follows:
density of wet mixture: 1.60-1.66 g/cm3
Density after hydration: 2.6 to 3.0g/cm3
Density of the coating: 3.0 to 3.2g/cm3
Porosity: 25 to 30 percent
After the coating is pressed, the coating is put into a dryer for natural drying for 46 to 52 hours, and then the coating is dried according to the following process: at room temperature 100-120 ℃ and preserving heat for 1-2 hours Keeping the temperature for 2 to 3 hours at the temperature of between 600 and 640 DEG C Keeping the temperature at 1000-1100 ℃ for 2-3 hours, cooling the mixture to 140-160 ℃ along with the furnace, and putting the mixture into a dryer for storage for later use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00110150 CN1124468C (en) | 2000-02-25 | 2000-02-25 | Magnesia crucible with calcium oxide coating and its making process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00110150 CN1124468C (en) | 2000-02-25 | 2000-02-25 | Magnesia crucible with calcium oxide coating and its making process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1310325A true CN1310325A (en) | 2001-08-29 |
| CN1124468C CN1124468C (en) | 2003-10-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00110150 Expired - Fee Related CN1124468C (en) | 2000-02-25 | 2000-02-25 | Magnesia crucible with calcium oxide coating and its making process |
Country Status (1)
| Country | Link |
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| CN (1) | CN1124468C (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7776155B2 (en) | 2002-03-29 | 2010-08-17 | Japan Super Quartz Corporation | Surface modified quartz glass crucible and its modification process |
| CN101967676A (en) * | 2002-03-29 | 2011-02-09 | 日本超精石英株式会社 | Surface modified quartz glass crucible and a process for modifying the crucible |
| CN101644534B (en) * | 2008-08-08 | 2011-06-22 | 中国科学院金属研究所 | Method for preparing large-capacity calcareous crucible for vacuum induction furnace |
| CN102517457A (en) * | 2011-12-30 | 2012-06-27 | 中原工学院 | Method utilizing graphite-clay crucible to smelt magnesium or magnesium alloy |
| CN102517456A (en) * | 2011-12-30 | 2012-06-27 | 中原工学院 | Method utilizing graphite-clay crucible to smelt magnesium or magnesium alloy |
| CN108218414A (en) * | 2016-12-21 | 2018-06-29 | 中国科学院金属研究所 | A kind of preparation method of high-capacity vacuum sensing smelting combined oxidation calcium crucible |
| 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 |
| CN111410562A (en) * | 2019-09-10 | 2020-07-14 | 包头稀土研究院 | Alkaline earth oxide crucible with rare earth oxyfluoride coating and preparation method thereof |
| CN114410994A (en) * | 2021-12-30 | 2022-04-29 | 北京科技大学 | Based on CaO-MgO-Al2O3Method for smelting nickel-based high-temperature alloy by using refractory material |
-
2000
- 2000-02-25 CN CN 00110150 patent/CN1124468C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7776155B2 (en) | 2002-03-29 | 2010-08-17 | Japan Super Quartz Corporation | Surface modified quartz glass crucible and its modification process |
| CN101967676A (en) * | 2002-03-29 | 2011-02-09 | 日本超精石英株式会社 | Surface modified quartz glass crucible and a process for modifying the crucible |
| CN101644534B (en) * | 2008-08-08 | 2011-06-22 | 中国科学院金属研究所 | Method for preparing large-capacity calcareous crucible for vacuum induction furnace |
| CN102517457A (en) * | 2011-12-30 | 2012-06-27 | 中原工学院 | Method utilizing graphite-clay crucible to smelt magnesium or magnesium alloy |
| CN102517456A (en) * | 2011-12-30 | 2012-06-27 | 中原工学院 | Method utilizing graphite-clay crucible to smelt magnesium or magnesium alloy |
| CN102517456B (en) * | 2011-12-30 | 2013-12-11 | 中原工学院 | Method utilizing graphite-clay crucible to smelt magnesium or magnesium alloy |
| CN102517457B (en) * | 2011-12-30 | 2013-12-11 | 中原工学院 | Method for utilizing graphite-clay crucible to smelt magnesium or magnesium alloy |
| CN108218414A (en) * | 2016-12-21 | 2018-06-29 | 中国科学院金属研究所 | A kind of preparation method of high-capacity vacuum sensing smelting combined oxidation calcium crucible |
| 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 |
| CN111410562A (en) * | 2019-09-10 | 2020-07-14 | 包头稀土研究院 | Alkaline earth oxide crucible with rare earth oxyfluoride coating and preparation method thereof |
| CN114410994A (en) * | 2021-12-30 | 2022-04-29 | 北京科技大学 | Based on CaO-MgO-Al2O3Method for smelting nickel-based high-temperature alloy by using refractory material |
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| Publication number | Publication date |
|---|---|
| CN1124468C (en) | 2003-10-15 |
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