CN105732061A - Lithium fluoride-doped zirconia crucible and method for producing lithium fluoride-doped zirconia crucible by hot-pressing sintering - Google Patents
Lithium fluoride-doped zirconia crucible and method for producing lithium fluoride-doped zirconia crucible by hot-pressing sintering Download PDFInfo
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- CN105732061A CN105732061A CN201610138136.8A CN201610138136A CN105732061A CN 105732061 A CN105732061 A CN 105732061A CN 201610138136 A CN201610138136 A CN 201610138136A CN 105732061 A CN105732061 A CN 105732061A
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- 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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
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Abstract
The invention discloses a lithium fluoride-doped zirconia crucible and a method for producing the lithium fluoride-doped zirconia crucible by hot-pressing sintering. The lithium fluoride-doped zirconia crucible is characterized in that 0.5-10 g of lithium fluoride is doped in every 100 g of zirconia; for hot-pressing sintering, particle size of the zirconia is 0.01-20 micrometers, and particle size of the lithium fluoride is 0.01-20 micrometers. The lithium fluoride-doped zirconia crucible has the advantages that the maximum service temperature is 1800 DEG C, high-temperature alloy materials containing active metals such as Al and Hf are subjected to vacuum melting at 1800 DEG C, and contents of gas elements such as oxygen, nitrogen and hydrogen are less than 5 ppm, 5 ppm and 1 ppm respectively.
Description
Technical field
The present invention relates to a kind of apparatus for melting metal, more particularly, refer to a kind of crucible that can be used in vacuum melting high temperature alloy and the method adopting hot pressed sintering crucible thereof.
Background technology
The crucible material that existing vacuum melting high temperature alloy uses is mainly calcium oxide, magnesium oxide etc., and the use temperature of crucible is generally 1200～1500 DEG C, has certain difficulty for super clean high temperature high vacuum melting.
Zirconium oxide (ZrO2) pottery has excellent heat-resisting, corrosion-resistant and high-temperature stability.Zirconic fusing point is more than 2600 DEG C, and is at high temperature difficult to react with some active metal, therefore can use as potential melting refractory material.
But zirconia ceramics moulding difficulty in commercial production, during sintering, change in volume is bigger, therefore zirconium oxide is only exist with additive form in traditional refractory material preparation technology, in zirconia ceramics, solid volume fraction is less than 25%, greatly reduces the use temperature of product.
General hot-press equipment (shown in Figure 1) includes sealing ring 1, stone grinder felt 2, heating coil 3, body of heater 4, pressed compact 5, stone grinder mould 6, power supply 7.Hot pressed sintering (Hot-Pressing, HP) is to apply certain external force (general pressure, between 10～40MPa, depends on the intensity that can bear with stone grinder mold materials) in sintering process simultaneously, makes material accelerate flowing, reset and densification.Usual hot pressed sintering temperature is lower than normal pressure-sintered temperature about 100 DEG C, depending on different objects and generate with or without liquid phase and different.Can preforming or powder is directly loaded in die cavity, technique is simple.The extrudate density that hot pressed sintering generally obtains is higher, more than the 99% of accessibility theory density, owing to sintering at a lower temperature, it is suppressed that the growth of crystal grain, and the sintered body crystal grain of gained is relatively thin, and has higher intensity.
Summary of the invention
It is an object of the invention to provide a kind of zirconium oxide doping lithium fluoride crucible that can be applicable to vacuum melting high activity metal or alloy and the technique that employing hot-pressing sintering method prepares zirconium oxide doping lithium fluoride crucible.
Disclosed a kind of zirconium oxide doping lithium fluoride crucible, mixed with the lithium fluoride of 0.5～10g in the zirconium oxide that composition is every 100g of described zirconium oxide doping lithium fluoride crucible.
Zirconium oxide doping lithium fluoride crucible uses temperature to be not more than 1800 DEG C
The present invention adopts hot-pressing sintering method to prepare specifically comprising the following steps that of zirconium oxide doping lithium fluoride crucible
The first step: slurrying material
The zirconium oxide of particle diameter 0.01～20 μm, the lithium fluoride of particle diameter 0.01～20 μm that are configured by according to target composition prepare slurry after mixing homogeneously with dehydrated alcohol；
Wherein the consumption of lithium fluoride be every 100g zirconium oxide in doped with the lithium fluoride of 0.5～10g, the consumption of dehydrated alcohol be every 100g zirconium oxide in add 0.05～0.1L；
Second step: dry base material
The slurry prepared in first step is dried in drying baker prepare blank, baking temperature 60～100 DEG C, drying time 8～15h；
3rd step: hot pressed sintering crucible
The blank that second step prepares is put in the die cavity of hot-press equipment, covers pressed compact, regulate pressure to 10～20MPa, 5～10 DEG C/min of heating rate, sintering temperature 1400～1600 DEG C, and under 1400～1600 DEG C of conditions of temperature, it is incubated 5～10h, the last demoulding prepares zirconium oxide doping lithium fluoride crucible.
Described zirconia powder material can also be the grating powder of multistage particle diameter, namely first order zirconia powder material particle diameter be 0.01～0.5 μm, second level zirconia powder material particle diameter be 0.5～2 μm, third level zirconia powder material particle diameter be 2～6 μm, fourth stage zirconia powder material particle diameter be 6～20 μm.
Owing to the zirconia powder material of different-grain diameter enters in oarse-grained space in mixed preparing process small particles, such that it is able to increase fine and close density, decrease the change in volume of high temperature sintering.
The advantage of zirconium oxide doping lithium fluoride crucible of the present invention is in that: (1) spendable temperature is for less than 1800 DEG C, it is adaptable to the smelting equipment of active metal or alloy is prepared in vacuum melting；(2) this zirconium oxide doping lithium fluoride crucible can improve the degree of purity of melt.
The present invention adopts the advantage that hot-pressing sintering method prepares zirconium oxide doping lithium fluoride crucible to be in that: (1) moulding is simple；(2) inner surface of crucible prepared is highly polished；(3) in sintering process, technological parameter is controlled.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of existing hot-press equipment.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Mixed with the lithium fluoride of 0.5～10g in the zirconium oxide that composition is every 100g of zirconium oxide doping lithium fluoride crucible of the present invention, it uses temperature to be not more than 1800 DEG C.
In the present invention, the zirconium oxide needed for preparing zirconium oxide doping lithium fluoride crucible is the fine powder of particle diameter 0.01～20 μm, and lithium fluoride is the fine powder of particle diameter 0.01～20 μm.
In the present invention, hot-pressing sintering method is adopted to prepare specifically comprising the following steps that of zirconium oxide doping lithium fluoride crucible
The first step: slurrying material
The zirconium oxide of particle diameter 0.01～20 μm, the lithium fluoride of particle diameter 0.01～20 μm that are configured by according to target composition prepare slurry after mixing homogeneously with dehydrated alcohol；
Wherein the consumption of lithium fluoride be every 100g zirconium oxide in doped with the lithium fluoride of 0.5～10g, the consumption of dehydrated alcohol is the zirconium oxide ZrO of every 100g2Middle addition 0.05～0.3L；
Second step: dry base material
The slurry prepared in first step is dried in drying baker prepare blank, baking temperature 60～100 DEG C, drying time 8～15h；
3rd step: hot pressed sintering crucible
The blank that second step prepares is put in the die cavity of hot-press equipment, covers pressed compact, regulate pressure to 10～20MPa, 5～10 DEG C/min of heating rate, sintering temperature 1400～1600 DEG C, and under 1400～1600 DEG C of conditions of temperature, it is incubated 5～10h, the last demoulding prepares zirconium oxide doping lithium fluoride crucible.
Above-mentioned prepared zirconium oxide doping lithium fluoride crucible is put in vacuum smelting equipment, and active metal block is put into crucible, in vacuum (vacuum 10～1 × 10-3Pa) or under inert atmosphere (argon, helium, neon), smelting temperature less than 1800 DEG C, melting high temperature alloy.
In the present invention, the zirconia powder material used can also be the grating powder of multistage particle diameter, namely first order zirconia powder material particle diameter be 0.01～0.5 μm, second level zirconia powder material particle diameter be 0.5～2 μm, third level zirconia powder material particle diameter be 2～6 μm, fourth stage zirconia powder material particle diameter be 6～20 μm.Owing to the zirconia powder material of different-grain diameter enters in oarse-grained space in mixed preparing process small particles, such that it is able to increase fine and close density, decrease the change in volume of high temperature sintering.
With specific embodiment, present disclosure is elaborated below.
Embodiment 1
Make a zirconium oxide doping lithium fluoride crucible that can hold 10kg high temperature alloy
Doped with the lithium fluoride of 184g in the zirconium oxide that target component is 3680g of this zirconium oxide doping lithium fluoride crucible.
The crucible step that employing hot pressed sintering prepares target component is as follows:
The first step: slurrying material
Particle diameter by according to target become assignment system 80% prepares slurry after the zirconium oxide of 4.8 μm, the lithium fluoride of particle diameter 5.0 μm of 80% are mixed homogeneously with 5L dehydrated alcohol；
Second step: dry base material
The slurry prepared in first step is dried at constant temp. drying box and prepares blank, dry temperature 60 C, drying time 15h；
3rd step: hot pressed sintering crucible
The blank that second step prepares is put in the die cavity of hot-press equipment, cover pressed compact, regulate pressure to 15MPa, 10 DEG C/min of heating rate, sintering temperature 1600 DEG C, and under 1600 DEG C of conditions of temperature, be incubated 8h；The last demoulding prepares the zirconium oxide doping lithium fluoride crucible of target component.
Above-mentioned target component zirconium oxide doping lithium fluoride crucible is adopted to carry out vacuum melting DD6 single crystal super alloy.The raw material bulk of 7kg is put into crucible, then crucible and material is arranged in true vacuum induction melting furnace in the lump；Regulate smelting technology parameter: be evacuated to 2.4 × 10-2Pa, smelting temperature 1800 DEG C, after refined, cooling is cast in graphite ingot mould, use Optima8000DVICP-OES inductively coupled plasma atomic emission elemental analyser detection alloy pig composition, oxygen content is less than 3ppm, and nitrogen content is less than 5ppm, and hydrogen content is less than 1ppm.
Embodiment 2
Make a zirconium oxide doping lithium fluoride crucible that can hold 200kg high temperature alloy
Doped with the lithium fluoride of 550g in the zirconium oxide that target component is 5500g of this zirconium oxide doping lithium fluoride crucible.
The crucible step that employing hot pressed sintering prepares target component is as follows:
The first step: slurrying material
Particle diameter by according to target become assignment system 90% prepares slurry with 10L dehydrated alcohol after the zirconium oxide of 15 μm, the lithium fluoride of 80% particle diameter 10 μm are mixed homogeneously；
Second step: dry base material
The slurry prepared in first step is dried at constant temp. drying box and prepares blank, dry temperature 80 DEG C, drying time 8h；
3rd step: hot pressed sintering crucible
The blank that second step prepares is put in the die cavity of hot-press equipment, covers pressed compact, regulate pressure to 15MPa, 5 DEG C/min of heating rate, sintering temperature 1400 DEG C, and under 1400 DEG C of conditions of temperature, it is incubated 5h, the last demoulding prepares the zirconium oxide doping lithium fluoride crucible of target component.
Above-mentioned target component zirconium oxide doping lithium fluoride crucible is adopted to carry out vacuum melting DZ125 high temperature alloy.The raw alloy bulk of 160kg is put into crucible, then crucible and material is arranged in vacuum induction melting furnace in the lump；Regulate smelting technology parameter: be evacuated to 1.9 × 10-2Pa, smelting temperature 1600 DEG C, it is poured into mild steel ingot mould after refine, adopts use Optima8000DVICP-OES inductively coupled plasma atomic emission elemental analyser detection alloy pig composition, oxygen content is less than 5ppm, and nitrogen content is less than 5ppm, and hydrogen content is less than 1ppm.
Claims (4)
1. a zirconium oxide doping lithium fluoride crucible, it is characterised in that: doped with the lithium fluoride of 0.5～10g in the zirconium oxide that composition is every 100g of described zirconium oxide doping lithium fluoride crucible.
2. zirconium oxide doping lithium fluoride crucible according to claim 1, it is characterised in that: zirconium oxide doping lithium fluoride crucible uses temperature to be not more than 1800 DEG C.
3. one kind adopts the method that hot-pressing sintering technique prepares the zirconium oxide doping lithium fluoride crucible described in claim 1, it is characterised in that have the following step:
The first step: slurrying material
The zirconium oxide of particle diameter 0.01～20 μm, the lithium fluoride of particle diameter 0.01～20 μm that are configured by according to target composition prepare slurry after mixing homogeneously with dehydrated alcohol；
Wherein the consumption of lithium fluoride be every 100g zirconium oxide in doped with the lithium fluoride of 0.5～10g, the consumption of dehydrated alcohol be every 100g zirconium oxide in add 0.05～0.1L；
Second step: dry base material
The slurry prepared in first step is dried in drying baker prepare blank, baking temperature 60～100 DEG C, drying time 8～15h；
3rd step: hot pressed sintering crucible
The blank that second step prepares is put in the die cavity of hot-press equipment, cover pressed compact；
Regulating pressure to 10～20MPa, 5～10 DEG C/min of heating rate, sintering temperature 1400～1600 DEG C, and be incubated 5～10h under 1400～1600 DEG C of conditions of temperature, the last demoulding prepares zirconium oxide doping lithium fluoride crucible.
4. the method for employing hot pressed sintering oxygenerating zirconium doping lithium fluoride crucible according to claim 3, it is characterized in that: the zirconia powder material used in the first step is the grating powder of multistage particle diameter, namely first order zirconia powder material particle diameter be 0.01～0.5 μm, second level zirconia powder material particle diameter be 0.5～2 μm, third level zirconia powder material particle diameter be 2～6 μm, fourth stage zirconia powder material particle diameter be 6～20 μm.
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| CN201610138136.8A CN105732061A (en) | 2016-03-11 | 2016-03-11 | Lithium fluoride-doped zirconia crucible and method for producing lithium fluoride-doped zirconia crucible by hot-pressing sintering |
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| CN201610138136.8A CN105732061A (en) | 2016-03-11 | 2016-03-11 | Lithium fluoride-doped zirconia crucible and method for producing lithium fluoride-doped zirconia crucible by hot-pressing sintering |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01139988A (en) * | 1987-11-26 | 1989-06-01 | Toshiba Corp | Crucible for melting metal |
| CN101239833A (en) * | 2008-03-12 | 2008-08-13 | 北京航空航天大学 | Yttrium oxide doping lithium fluoride crucible and producing method thereof by using hot pressing sintering |
| CN101605736B (en) * | 2007-05-15 | 2013-02-06 | 特莱巴赫工业有限公司 | Yttria-based refractory composition |
| CN102965529A (en) * | 2012-11-30 | 2013-03-13 | 上海大学 | Preparation method of short-process titanium alloy Ti-Ni-Nb |
| CN105236980A (en) * | 2015-11-19 | 2016-01-13 | 中国工程物理研究院化工材料研究所 | ZrO2-LiF-codoped vacuum sintering method for lutetium oxide transparent ceramic |
-
2016
- 2016-03-11 CN CN201610138136.8A patent/CN105732061A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01139988A (en) * | 1987-11-26 | 1989-06-01 | Toshiba Corp | Crucible for melting metal |
| CN101605736B (en) * | 2007-05-15 | 2013-02-06 | 特莱巴赫工业有限公司 | Yttria-based refractory composition |
| CN101239833A (en) * | 2008-03-12 | 2008-08-13 | 北京航空航天大学 | Yttrium oxide doping lithium fluoride crucible and producing method thereof by using hot pressing sintering |
| CN102965529A (en) * | 2012-11-30 | 2013-03-13 | 上海大学 | Preparation method of short-process titanium alloy Ti-Ni-Nb |
| CN105236980A (en) * | 2015-11-19 | 2016-01-13 | 中国工程物理研究院化工材料研究所 | ZrO2-LiF-codoped vacuum sintering method for lutetium oxide transparent ceramic |
Non-Patent Citations (1)
| Title |
|---|
| 吴树森等: "《有色金属熔炼入门与精通》", 31 May 2014, 机械工业出版社 * |
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Application publication date: 20160706 |