CN104311041A - Beryllium oxide crucible for smelting pure beryllium, and preparation method thereof - Google Patents
Beryllium oxide crucible for smelting pure beryllium, and preparation method thereof Download PDFInfo
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- CN104311041A CN104311041A CN201410148790.8A CN201410148790A CN104311041A CN 104311041 A CN104311041 A CN 104311041A CN 201410148790 A CN201410148790 A CN 201410148790A CN 104311041 A CN104311041 A CN 104311041A
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- 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
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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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
- C04B35/08—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 beryllium 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
- 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
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
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- Crucibles And Fluidized-Bed Furnaces (AREA)
Abstract
The invention relates to a beryllium oxide crucible for smelting pure beryllium, and a preparation method thereof. The beryllium oxide crucible for smelting the pure beryllium is formed by using calcined beryllium oxide as a main material, 0.1%-0.5% by weight of phosphoric acid and 3%-10% by weight of pure water as auxiliary materials; mixing the above materials uniformly under stirring; tamping and sintering. According to the invention, calcined beryllium oxide is used as a raw material; phosphoric acid and pure water are used as binding agents; and the beryllium oxide crucible for smelting the pure beryllium is prepared by adopting a tamping forming method. The process flow is short; the production method is simple; a preparation period is short; the prepared pure beryllium crucible has good suddenly-changing temperature resistance and can fully guarantee the purity of beryllium ingots.
Description
Technical field
The invention belongs to smelting non-ferrous metal equipment technical field, particularly relate to a kind of pure beryllium melting beryllia crucible and preparation method thereof.
Background technology
Pure beryllium chemical property is active, after fusing, at high temperature very easily with other ceramic crucible generation replacement(metathesis)reaction, thus introduce impurity, reduce the purity of beryllium ingot.Therefore the crucible of the pure beryllium of melting must meet following condition: high temperature resistant, refractoriness under load wants high, and when smelting metal, crucible can not feel like jelly fusing; Crucible material does not pollute metal, and slag resistance will be got well, not by slag corrosion; Crucible heat-resistant knocking stability will be got well; Crucible dimensional stability when high temperature will be got well, indeformable.
Beryllium oxide due to fusing point high, thermal expansivity is little, and chemical stability is good, is ideal material prepared by pure beryllium crucible for smelting.At present, domestic conventional beryllia crucible preparation method is that Slurry casting and powder pressing forming are through high-temperature sintering process.The weak point of this method is: technical process is long, production method is complicated, preparation cycle is long, the crucible heat-resistant knocking stability of preparation is poor.
Summary of the invention
Object of the present invention is just the defect overcoming above-mentioned prior art, provides a kind of technical process short, and production method is simple, and preparation cycle is short, simultaneously good, the pure beryllium melting beryllia crucible that ensures melting material purity of heat impact strength;
Another object of the present invention is to provide the preparation method of above-mentioned pure beryllium melting beryllia crucible.
Technical scheme taked for achieving the above object is:
A kind of pure beryllium melting beryllia crucible, to it is characterized in that with calcined oxide beryllium for major ingredient, and be aided with the phosphoric acid of 0.1% ~ 0.5% and the pure water uniform stirring of 3% ~ 10% and make sintering firm by ramming and form, said ratio by weight percentage.
Described calcined oxide beryllium is mixed according to the weight proportion of 25%:55%:20% at 5 ~ 10mm, 2 ~ 5mm and the calcined oxide beryllium particle that is less than 2mm respectively by particle diameter.
A kind of preparation method of pure beryllium melting beryllia crucible; it is characterized in that its processing step is: the calcined oxide beryllium particle first particle diameter being respectively 5 ~ 10mm, 5 ~ 10mm according to the weight proportion of 25%:55%:20% and being less than 2mm is mixed into major ingredient; then the phosphoric acid of 0.1% ~ 0.5% of its weight is added and the pure water of 3% ~ 10% is mixed thoroughly; adopt and make shaping mode ramming firm by ramming, finally sinter.
Described calcined oxide beryllium particle refer to beryllium oxide powder added weight 10% pure water, repressed, dry, obtain after calcining and fragmentation.
Described compacting adopts cold isostatic press compacting, controls pressing pressure to 800kg.
Describedly make shaping step firm by ramming and be: first inside intermediate frequency furnace induction coil, spread woven asbesto, graphite fuse is put in centre, and chassis adds chassis and turns, and is filled in space afterwards by raw material, mechanical ramming.
Temperature during described sintering controls: 5Kw/ insulation 0.5h → 10Kw/ insulation 1.0h → 15Kw/ insulation 1.0h → 20Kw/ is incubated 1.0h → 30Kw/ and is incubated 2.5h.
The present invention with calcined oxide beryllium for raw material, be aided with phosphoric acid and pure water as binding agent, employing is made shaping method firm by ramming and is prepared pure beryllium melting beryllia crucible, its technical process is short, production method is simple, and preparation cycle is short, prepared pure beryllium crucible, heat impact strength is good, fully can ensure the purity of beryllium ingot.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail.
Embodiment 1
1, the preparation of beryllium oxide calcining material
In 50kg beryllium oxide powder, add the pure water of weight 5kg, dress jacket, adopt cold isostatic press to be pressed, control pressing pressure 800kg (0 ~ 800kg pressurize 1 hour, more than 800kg pressurize 30 minutes.)。Calcining: install in plumbago crucible by the raw material suppressed, sinter at medium-frequency induction furnace, increases the loose density of oxide skin.Calcining process is:
calcining material is carried out coarse breaking and fine crushing respectively, screen with the sieve of three kinds of specifications afterwards, the specification of sieve is respectively 5 centimetres, 2 centimetres, is less than 2 centimetres, obtain the particulate material of three kinds of particle size range, i.e. particle diameter 5 ~ 10 ㎜ particulate material, particle diameter 2 ~ 5 ㎜ particulate material and particle diameter ﹤ 2 ㎜ particulate material.
2, the preparation of beryllia crucible
Batching: according to the weight proportion of 25%:55%:20% by three kinds of particle diameters: the beryllium oxide particulate material of particle diameter 5 ~ 10 ㎜, particle diameter 2 ~ 5 ㎜ and particle diameter ﹤ 2 ㎜ is mixed into major ingredient, then the phosphoric acid (analytical pure) adding 0.1% of major ingredient weight makees binding agent, add the pure water of 10% of major ingredient weight again, stir.
Make firm by ramming shaping: carry out in intermediate frequency furnace.Serve as a contrast with woven asbesto inside the intermediate frequency furnace induction coil handled well, graphite fuse is put in centre, and bottom adds chassis brick.Above-mentioned compound ramming crucible between the space of chassis brick and graphite fuse and woven asbesto and graphite fuse, requires tamping.
Ruhmkorff coil: beryllium melting intermediate frequency furnace ruhmkorff coil, conduction produces induced current, sinters for crucible.
Graphite core: be inductor during medium-frequency induction furnace sintering, for responding to generation heat.Can produce the electric current of constantly change after ruhmkorff coil energising, the current induced magnetic field of change, can respond to and produce swirl shape electric current (eddy current) on graphite core, electric current passes through graphite core (resistance) thus produces heat.
Woven asbesto: mainly heat insulation, prevent ruhmkorff coil overheated, burn.Be conducive to the adhesion preventing beryllium oxide and ruhmkorff coil simultaneously.
Graphite core and beryllium oxide isolated: be wound around kraft paper on graphite core, again with rubber adhesive tape fixes (three kind materials in crucible sintering process burn removal) after being fastened with elongated cloth bag.For being separated of crucible and graphite core.
Crucible ramming equipment: electric pick.Circular arc impact head.
Sintering: with the control temperature of rising progressively of power during crucible sintering, temperature control flow: 5Kw/ insulation 0.5h → 10Kw/ insulation 1.0h → 15Kw/ insulation 1.0h → 20Kw/ is incubated 1.0h → 30Kw/ and is incubated 2.5h.Heating, cooling process entails evenly, steadily, thermograde is little avoids shock heating quenching.
Deposit: after terminating, have a power failure and take out graphite fuse, the crucible sintered should remain on vacuum state and preserve.
Claims (7)
1. a pure beryllium melting beryllia crucible, to it is characterized in that with calcined oxide beryllium for major ingredient, and be aided with the phosphoric acid of 0.1% ~ 0.5% and the pure water uniform stirring of 3% ~ 10% and make sintering firm by ramming and form, said ratio by weight percentage.
2., according to pure beryllium melting beryllia crucible according to claim 1, it is characterized in that described calcined oxide beryllium is mixed according to the weight proportion of 25%:55%:20% at 5 ~ 10mm, 2 ~ 5mm and the calcined oxide beryllium particle that is less than 2mm respectively by particle diameter.
3. the preparation method of a pure beryllium melting beryllia crucible; it is characterized in that its processing step is: the calcined oxide beryllium particle first particle diameter being respectively 5 ~ 10mm, 5 ~ 10mm according to the weight proportion of 25%:55%:20% and being less than 2mm is mixed into major ingredient; then the phosphoric acid of 0.1% ~ 0.5% of its weight is added and the pure water of 3% ~ 10% is mixed thoroughly; adopt and make shaping mode ramming firm by ramming, finally sinter.
4. according to the preparation method of pure beryllium melting beryllia crucible according to claim 3, it is characterized in that described calcined oxide beryllium particle refer to beryllium oxide powder added weight 10% pure water, repressed, dry, obtain after calcining and fragmentation.
5., according to the preparation method of pure beryllium melting beryllia crucible according to claim 4, it is characterized in that described compacting adopts cold isostatic press compacting, control pressing pressure to 800kg.
6. according to the preparation method of pure beryllium melting beryllia crucible according to claim 3, making shaping step described in it is characterized in that firm by ramming is: first inside intermediate frequency furnace induction coil, spread woven asbesto, graphite fuse is put in centre, and chassis adds chassis and turns, afterwards raw material are filled in space, mechanical ramming.
7. according to the preparation method of pure beryllium melting beryllia crucible according to claim 3, temperature control when it is characterized in that described sintering is: 5Kw/ is incubated 0.5h → 10Kw/ insulation 1.0h → 15Kw/ insulation 1.0h → 20Kw/ and is incubated 1.0h → 30 Kw/insulation 2.5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410148790.8A CN104311041A (en) | 2014-04-15 | 2014-04-15 | Beryllium oxide crucible for smelting pure beryllium, and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410148790.8A CN104311041A (en) | 2014-04-15 | 2014-04-15 | Beryllium oxide crucible for smelting pure beryllium, and preparation method thereof |
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| CN104311041A true CN104311041A (en) | 2015-01-28 |
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| CN201410148790.8A Pending CN104311041A (en) | 2014-04-15 | 2014-04-15 | Beryllium oxide crucible for smelting pure beryllium, and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109824370A (en) * | 2019-03-21 | 2019-05-31 | 中国工程物理研究院材料研究所 | A kind of beryllium alumin(i)um alloy induction melting composite multi-layer crucible and preparation method thereof |
| WO2020214755A1 (en) | 2019-04-17 | 2020-10-22 | Materion Corporation | Crucibles and compositions and processes for making same |
| CN112125682A (en) * | 2020-08-21 | 2020-12-25 | 宁波长振铜业有限公司 | Furnace striking material for melting channel of regenerative brass power frequency induction furnace and use method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1365948A (en) * | 2001-11-16 | 2002-08-28 | 水口山有色金属有限责任公司第六冶炼厂 | Process for preparing industrial beryllium oxide by sulfuric acid method |
| CN202613969U (en) * | 2012-04-28 | 2012-12-19 | 广州金凯新材料有限公司 | Lining of intermediate frequency furnace |
| CN103088205A (en) * | 2011-11-02 | 2013-05-08 | 峨眉山市中山铁合金冶炼有限公司 | Beryllium oxide production process |
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2014
- 2014-04-15 CN CN201410148790.8A patent/CN104311041A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1365948A (en) * | 2001-11-16 | 2002-08-28 | 水口山有色金属有限责任公司第六冶炼厂 | Process for preparing industrial beryllium oxide by sulfuric acid method |
| CN103088205A (en) * | 2011-11-02 | 2013-05-08 | 峨眉山市中山铁合金冶炼有限公司 | Beryllium oxide production process |
| CN202613969U (en) * | 2012-04-28 | 2012-12-19 | 广州金凯新材料有限公司 | Lining of intermediate frequency furnace |
Non-Patent Citations (2)
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| 刘崇志译: "《铍》", 31 March 1959, 冶金工业出版社 * |
| 胡宝玉等: "《特种耐火材料实用技术手册》", 30 June 2004, 冶金工业出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109824370A (en) * | 2019-03-21 | 2019-05-31 | 中国工程物理研究院材料研究所 | A kind of beryllium alumin(i)um alloy induction melting composite multi-layer crucible and preparation method thereof |
| CN109824370B (en) * | 2019-03-21 | 2021-10-15 | 中国工程物理研究院材料研究所 | Composite multilayer crucible for beryllium-aluminum alloy induction smelting and preparation method thereof |
| WO2020214755A1 (en) | 2019-04-17 | 2020-10-22 | Materion Corporation | Crucibles and compositions and processes for making same |
| CN112125682A (en) * | 2020-08-21 | 2020-12-25 | 宁波长振铜业有限公司 | Furnace striking material for melting channel of regenerative brass power frequency induction furnace and use method |
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Application publication date: 20150128 |