CN2856899Y - Melting crucible of Ti and Ti alloy - Google Patents
Melting crucible of Ti and Ti alloy Download PDFInfo
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- CN2856899Y CN2856899Y CN 200620053250 CN200620053250U CN2856899Y CN 2856899 Y CN2856899 Y CN 2856899Y CN 200620053250 CN200620053250 CN 200620053250 CN 200620053250 U CN200620053250 U CN 200620053250U CN 2856899 Y CN2856899 Y CN 2856899Y
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- titanium
- boron nitride
- barrier layer
- lining
- titanium alloy
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Abstract
The utility model relates to a titanium and titanium alloy melting kettle, comprising a casing, a boron nitride lining, and a barrier layer, wherein the boron nitride lining is enclosed by the casing, and the barrier layer is attached to the inner surface of the boron nitride lining in contact with the titanium and titanium alloy liquid. The melting kettle has no reaction with the titanium, can be maintained conveniently, and has a long service life, and the molten bath has a good fluidity, especially, the boron and nitrogen increase can be reduced because of the barrier layer, and the boron content or nitrogen content in the titanium and titanium alloy can be controlled below 100ppm, thereby the titanium alloy quality can be improved efficiently.
Description
Technical Field
The utility model belongs to a metal melting crucible, in particular to a titanium and titanium alloy melting crucible.
Background
Because of the high melting point and the very active chemical properties of titanium, liquid titanium can react with almost all crucible refractories such as zirconia, magnesia, silica and alumina during melting, thus causing the melting to be impossible with vacuum induction melting using crucibles made of conventional refractories. At present, titanium and titanium alloy are smelted in industry by adopting a vacuum consumable electrode arc skull furnace and forced water-cooling copper crucible for cooling. When the vacuum arc skull furnace is used for smelting, a thin layer of skull is firstly solidified on the wall of a copper crucible, so that the effects of protecting titanium liquid from being polluted by crucible materials and insulating heat are achieved, and a molten pool is formed in the crucible. Because the water-cooled copper crucible is cooled quickly and a skull is formed, the temperature field of the titanium liquid is not uniform, and the retention time of the titanium alloy in the liquid state is short, so that the components of the cast titanium alloy are not uniform after pouring. The non-uniform components greatly affect the performance of the alloy,for example, the phase change point of the titanium-nickel shape memory alloy is sensitive to the components. Compared with the vacuum induction furnace smelting, the vacuum arc skull melting furnace smelting has large energy consumption, and the power consumption for smelting the titanium alloy is 40-60 kw/kg. In order to solve the above problems, calcium oxide has been proposed as a melting crucible for titanium and titanium alloys. However, calcium oxide is difficult to sinter and form, a calcium oxide crucible is easy to hydrolyze in air, and in addition, the oxygen content in the titanium alloy smelted by the calcium oxide crucible is increased, which affects the performance of the titanium alloy. The inventor in Chinese patent ZL200410025119.0 discloses a titanium and titanium alloy melting crucible material and a manufacturing method for making a crucible by the material, boron nitride and a proper amount of fluxing agent are used as raw materials, the raw materials are pressed into a crucible blank by cold isostatic pressing, and the crucible blank is sintered for 1 hour at 1800 ℃ to obtain a finished melting crucible product, and the finished melting crucible product has good effect on laboratory scale application, and has the advantages of no reaction with titanium and no bonding with alloy at high temperature; low energy consumption, uniform alloy components after smelting and pouring and stable performance. However, the above-mentioned technology disclosed in the patent cannot meet the requirement of industrial production because of the technical solution of manufacturing the monolithic crucible by cold isostatic pressing and sintering molding of boron nitride and proper amount of flux, because the volume of the melting crucible required for industrial production is large, the technology disclosed in patent ZL200410025119.0 is difficult to manufacture, and the reason is that: (1) in the industrial production, the crucible (generally in ton unit) is large in volume, and the equipment for cold isostatic pressing, sintering and the like required for the production of the entire boron nitride crucible is expensive and needs to be manufactured in particular. (2) The integrally manufactured boron nitride crucible is expensive, and once the crucible is damaged and cannot be repaired, the crucible needs to be integrally replaced, so that the economic cost is not low. (3) And cracks are easy to generate in the manufacturing and using processes of the integrally manufactured boron nitride crucible.
In addition, Zhao Feng Ming et al in the literature "application of pyrolytic boron nitride crucible in special melting" and "growth and performance of pyrolytic boron nitride crucible material" 2 article disclose a preliminary application effect of pyrolytic boron nitride crucible in titanium and titanium alloy melting and a manufacturing method of pyrolytic boron nitride crucible. Pyrolytic Boron Nitride (PBN) crucibles have many unique properties, such as: the pyrolytic boron nitride crucible has excellent chemical and thermal stability, the intensity of the pyrolytic boron nitride crucible is improved along with the rise of the temperature when the pyrolytic boron nitride crucible is sublimated at 3000 ℃, and the intensity reaches the maximum value when the temperature is 2200 ℃; the acid, alkali, salt and organic reagent are resistant at room temperature, so that the storage is convenient, and the acid resistance is realized at high temperature; the pyrolytic boron nitride crucible has high density and no air holes, and the density of the pyrolytic boron nitride crucible is close to the theoretical density (2.27 g/cm) of the material3) The molten metal is difficult to permeate into the crucible wall, when the small crucible is used for smelting titanium and titanium alloy, the molten metal can be easily poured out even when the small crucible is cooled to room temperature along with the furnace, the inner wall of the crucible is smooth and clean, no bonding phenomenon exists, no residue is left, the crucible is easy to clean and can be repeatedly used; compared with a boron nitride crucible sintered and formed after cold isostatic pressing, the pyrolytic boron nitride crucible has obvious anisotropy in the aspects of mechanical property, thermal property, electrical property and the like, and simultaneously has good microwave and infrared ray transmitting performance, the difference of the thermal conductivity in the deposition direction and the direction vertical to the deposition surface is about 20 times, namely the surface of the crucible is a good thermal conductor, and the direction vertical to the surface of the crucible is a heat insulator, when the crucible is used for smelting titanium, the thermal field in the crucible is uniform,the heat is difficult to be dissipated through the crucible wall, so that the heat preservation performance is improved, and the electric power can be saved by about one half; in addition, the PBN crucible has good thermal shock resistance, and no crack is generated when the PBN crucible is directly put into water at 2000 ℃.
Like the technique disclosed in the chinese patent ZL200410025119.0, zhao fengming et al disclose a boron nitride crucible integrally manufactured from pyrolytic boron nitride crucible in the documents "application of pyrolytic boron nitride crucible in special melting" and "growth and performance of pyrolytic boron nitride crucible material", which is only suitable for laboratory and small-batch production, and all have the three disadvantages of the integrally manufactured boron nitride crucible discussed above in industrial scale production; meanwhile, no matter pyrolytic boron nitride or sintered boron nitride is adopted as a melting crucible of titanium and titanium alloy, nitrogen and boron increase phenomena exist in the melted titanium and titanium alloy to different degrees, the content of nitrogen and boron in the titanium and titanium alloy is too high,brittleness is caused, and the performance of the alloy is influenced.
Disclosure of Invention
An object of the utility model is to provide a titanium and titanium alloy smelt crucible can satisfy industrialization, big volume, low cost, easy maintenance, longe-lived requirement to nitrogen increase and boron increase phenomenon in the alloy when can effectively reduce titanium and titanium alloy and smelt.
The crucible comprises a shell, a boron nitride lining and a barrier layer, wherein the shell coats the boron nitride lining, and the barrier layer is attached to the inner surface of the boron nitride lining, which is in contact with titanium and titanium alloy liquid.
The barrier layer is a reaction layer containing a compound between titanium and boron or a compound between titanium and nitrogen formed by aging treatment between titanium and boron nitride.
-the barrier layer is a layer containing a high melting point substance TiB2Or a reaction barrier layer of TiB.
The barrier layer is a high-melting-point substance TiB formed by embedding a boron nitride containing lining in titanium powder or titanium powder and catalyst mixed powder through high-temperature interdiffusion2Or a reaction barrier layer of TiB.
The barrier layer is TiB containing high-melting point substance formed by spraying metallic titanium or a mixed coating of metallic titanium and a catalyst on a lining containing boron nitride and then performing high-temperature interdiffusion2Or a reaction barrier layer of TiB.
The thickness of the barrier layer is between 0.05mm and 0.5mm, and the preferable thickness is 0.15 mm to 0.35 mm.
-the boron nitride liner is a bulk sintered boron nitride liner or a bulk manufactured pyrolytic boron nitride liner.
-the boron nitride lining is a cup-shaped structure formed by a single layer of bricks built up by sintering boron nitride bricks or a cup-shaped structure formed by a double layer of bricks or a cup-shaped structure formed by more than two layers of bricks.
-the boron nitride lining is a cup-shaped structure formed by a single layer of bricks built up from a stack of pyrolytic boron nitride bricks, or a cup-shaped structure formed by double layers of bricks, or a cup-shaped structure formed by more than two layers of bricks.
The boron nitride lining is a cup-shaped structure formed by single-layer bricks built by boron nitride single-crystal bricks or a cup-shaped structure formed by double-layer bricks or a cup-shaped structure formed by more than two layers of bricks.
The shell is a shell which is matched with the shape of the boron nitride lining and has the functions of heat insulation, heat preservation and force bearing.
The utility model has the advantages that:
through ageing treatment, a reaction layer containing titanium and boron compounds or titanium and nitrogen compounds with the thickness of 0.05-0.50 mm, especially TiB, is formed on the inner surface of the boron nitride lining, which is in contact with the titanium and titanium alloy liquid2The TiB reaction layer can effectively prevent boron and nitrogen from diffusing into titanium and titanium alloy liquid, effectively reduces the phenomena of boron increase and nitrogen increase when the boron nitride crucible is used for smelting titanium and titanium alloy, and improves the quality of the titanium and titanium alloy.
Drawings
FIG. 1 is a schematic view of a crucible according to the present invention.
Fig. 2 is a sectional view a-a of fig. 1.
Fig. 3 is a schematic structural view of a crucible of the present invention, the inner lining of which is built by double-layer boron nitride bricks.
Fig. 4 is a schematic structural view of a crucible of the present invention with a lining built up by three layers of boron nitride bricks.
FIG. 5 is a schematic view of a crucible of the present invention having a boron nitride liner produced by a bulk sintering process.
Fig. 6 is a schematic view of a crucible of the present invention employing an integrally formed pyrolytic boron nitride liner.
In the above figures: 1 is the shell, 2 is the boron nitride lining, 3 is the barrier layer.
Detailed Description
1.1 manufacture of sintered boron nitride bricks
Mixing boron nitride powder or boron nitride powder and proper amount of flux uniformly, making brick-shaped blank in mould by cold isostatic pressing, and sintering at 1800 deg.C for 1-2 hr to obtain sintered boron nitride brick.
The fluxing agents used in sintering the boron nitride bricks respectively adopt zirconium oxide, magnesium oxide and boron oxide, such as: the weight percent white ratio of 0.5 percent of zirconium oxide, 1 percent of magnesium oxide and 1.5 percent of boron oxide can be used as a fluxing agent for sintering the boron nitride brick.
1.2 production of bulk sintered boron nitride liners
The basic process is the same as the manufacturing process of the 1.1 sintered boron nitride brick, except that the mould adopted in the cold isostatic pressing blank making process is different, the blank is directly and integrally pressed into a cup shape required by the crucible, and then the blank is sintered and molded at high temperature.
1.3 manufacture of pyrolytic boron nitride bricks
The method comprises the following steps of manufacturing a blank of the pyrolytic boron nitride brick by adopting a chemical vapor deposition process, and then machining the blank into a required shape and size to obtain the pyrolytic boron nitride brick, wherein the method specifically comprises the following steps:
high-purity raw material gas BCl3And NH3Mixing the raw materials according to a certain proportion, introducing the mixture into a high-temperature reaction chamber, wherein the temperature of the reaction chamber is up to 2000 ℃, and the mixed gas is in the reaction chamber and is carried out according to the following chemical reaction equation:
during the growth of Pyrolytic Boron Nitride (PBN) materials, one is always accustomed to constantly depositing snow, i.e. hexagonal BN flakes grown in reaction, on a heated graphite substrate (mandrel) and, over time, thickening the deposited layer to form a shell of pyrolytic boron nitride, and removing the shell to obtain a separate, pure pyrolytic boron nitride blank. Pyrolytic boron nitride has good machining performance, and the pyrolytic boron nitride blank is processed into the shape and the size required by the picture paper, and the utility model discloses required pyrolytic boron nitride brick is obtained.
Chemical vapor deposition of pyrolytic boron nitride materials is simple and complex. The equipment is simple, the principle is simple, and the operation is simple; however, the process is complicated in influencing factors, such as the raw material intake mode, the charging mode, the size and geometry of the hearth, the arrangement position and mode of the core mold and the like, which all affect the vapor deposition, and in severe cases, the whole furnace is scrapped. However, the main parameters of vapor deposition are the temperature of the substrate, the pressure in the furnace and the gas flow ratio. The temperature is 1800-1900 ℃, the pressure in the furnace is 1-2 mmHg, the flow rate of the gas depends on the size of the furnace space and the requirement of the sediment, and a high-temperature process is usually adopted for growing the pyrolytic boron nitride brick used for the crucible lining.
The boron nitride brick can have different geometric shapes, especially can be designed into the shape that can be mutually positioned in concave-convex matching, not only can be conveniently piled into a lining, but also is convenient to replace after the boron nitride brick is damaged.
1.4 manufacture of bulk pyrolytic boron nitride liners
The basic process is the same as the manufacturing process of the 1.3 pyrolytic boron nitride brick, except that a graphite mold adopted in chemical vapor deposition is different, and a graphite male mold is directly adopted to form a cup-shaped pyrolytic boron nitride lining required by the crucible.
1.5 manufacture of the outer Shell
The shell can be made of refractory materials (such as graphite, calcium oxide, zirconium oxide and the like) to achieve the functions of heat insulation, heat preservation and bearing, and the shape of the shell is matched with that of boron nitride. The most common housing is made of graphite.
1.6 formation of barrier layer process example 1
The reaction time can be shortened by embedding the whole sintered boron nitride lining or the whole pyrolytic boron nitride lining in metal titanium powder with the particle size of below-100 meshes or metal titanium powder with the particle size of below-100 meshes and a catalyst, and selecting boride as the catalyst. Sintering at 1000-1600 deg.c for 2-30 hr, and interdiffusion to form TiB on the lining of boron nitride2Is predominantly or TiB2Washing the high-melting-point reaction barrier layer with TiB as a main body for 1-2 times by using titanium liquid to obtain TiB with the thickness of about 0.05-0.5 mm2A reaction barrier layer of TiB, preferably 0.15-0.35 mm thick.
For the boron nitride lining piled up by the boron nitride bricks, whether the boron nitride bricks are sintered or pyrolytic boron nitride bricks, the boron nitride lining piled up by the boron nitride bricks is firstly arranged in a graphite shell according to the design drawing, then the lining piled up by the boron nitride bricks is filled with metal titanium powder below-100 meshes or metal titanium powder below-100 meshes and a catalyst, the sintering is carried out for 2-30 hours at the temperature of 1000-1600 ℃, and TiB can be formed on the boron nitride lining through mutual diffusion2Is predominantly or TiB2Washing the high-melting-point reaction barrier layer with TiB as a main body for 1-3 times by using titanium liquid to obtain TiB with the thickness of about 0.05-0.5 mm2A reaction barrier layer of TiB, preferably 0.15-0.35 mm thick.
1.7 formation of barrier layer process example 2
Whether for bulk boron nitrideThe lining is also a lining piled up by boron nitride bricks, a layer of metallic titaniumor a mixed coating of the metallic titanium and a catalyst is sprayed on the inner surface of the lining contacted with titanium and titanium alloy liquid by adopting a plasma spraying technology, then sintering is carried out for 2-30 hours at 1000-1600 ℃, and TiB can be formed on the boron nitride lining by mutual diffusion2Is predominantly or TiB2Washing the high-melting-point reaction barrier layer with TiB as a main body for 1-3 times by using titanium liquid to obtain TiB with the thickness of about 0.05-0.5 mm2A reaction barrier layer of TiB, preferably 0.15-0.35 mm thick.
1.8 production of melting crucible for titanium and titanium alloy
The boron nitride lining with the barrier layer is assembled in the shell according to the design requirement of the crucible drawing, thus obtaining the titanium and titanium alloy smelting crucible of the utility model.
The use of a single or double or multi-layer boron nitride liner, the thickness of the barrier layer, and the material used and the support strength of the outer shell may be determined by the size, capacity, composition of the titanium alloy being melted primarily, of the particular crucible.
1.9 application of titanium and titanium alloy smelting crucible
The crucible of the utility model is arranged in a vacuum induction furnace to smelt titanium alloy, and the average power consumption is 2-3 kw/kg. When in smelting, the lining of the crucible does not react with titanium at high temperature, does not bond with alloy, has good molten pool fluidity, has uniform alloy components after smelting and pouring, has stable performance, particularly effectively reduces boron increase and nitrogen increase due to the existence of a barrier layer, can control the boron content or the nitrogen content of the smelted titanium and the titanium alloy to be below 100ppm, and effectively improves the quality of the titanium alloy.
It should be noted that the structures disclosed and described herein may be replaced by other structures having the same effect, and the embodiments described herein are not the only structures for implementing the present invention. Although preferred embodiments of the present invention have been shown and described herein, it will be understood by those skilled in the art that these embodiments are by way of example only and that numerous changes, modifications and substitutions may be made without departing from the invention in its broader aspects and, therefore, the invention is to be limited only by the spirit and scope of the appended claims.
Claims (11)
1. The titanium and titanium alloy smelting crucible is characterized by comprising a shell (1), a boron nitride lining (2) and a barrier layer (3), wherein the shell (1) coats the boron nitride lining (2), and the barrier layer (3) is attached to the inner surface, in contact with titanium and titanium alloy liquid, of the boron nitride lining (2).
2. The melting crucible of titanium and titanium alloy as set forth in claim 1, wherein the barrier layer (3) is a reaction layer containing a compound between titanium and boron or a compound between titanium and nitrogen formed by aging treatment between titanium and boron nitride.
3. A titanium and titanium alloy melting crucible according to claim 1 or 2, wherein the barrier layer (3) is TiB containing a high melting point substance2Or a reaction barrier layer of TiB.
4. The melting crucible of claim 1 or 2, wherein the barrier layer (3) is a TiB containing high melting point material formed by embedding a boron nitride containing lining in titanium powder or titanium powder and catalyst mixed powder through high-temperature interdiffusion2Or a reaction barrier layer of TiB.
5. The melting crucible of claim 1 or 2, wherein the barrier layer (3) is TiB containing high melting point material formed by spraying metallic titanium or a mixed coating of metallic titanium and a catalyst on a lining containing boron nitride and then performing high-temperature interdiffusion2Or a reaction barrier layer of TiB.
6. A titanium and titanium alloy melting crucible according to claim 1 or 2, wherein the thickness of the barrier layer (3) is between 0.05mm and 0.5mm, preferably between 0.15 mm and 0.35 mm.
7. A titanium and titanium alloy melting crucible according to claim 1, wherein the boron nitride lining (2) is a bulk sintered boron nitride lining or a bulk manufactured pyrolytic boron nitride lining.
8. The titanium and titanium alloy melting crucible according to claim 1, wherein the boron nitride lining (2) is a cup-shaped structure formed by a single layer brick built by a sintered boron nitride brick stack, a cup-shaped structure formed by a double layer brick, or a cup-shaped structure formed by more than two layers of bricks.
9. A titanium and titanium alloy melting crucible according to claim 1, wherein the boron nitride lining (2) is a cup-shaped structure formed by a single layer brick built up by a stack of pyrolytic boron nitride bricks or a cup-shaped structure formed by a double layer brick or a cup-shapedstructure formed by more than two layers of bricks.
10. The titanium and titanium alloy melting crucible according to claim 1, wherein the boron nitride lining (2) is a cup-shaped structure formed by single-layer bricks built by boron nitride single-crystal bricks, a cup-shaped structure formed by double-layer bricks or a cup-shaped structure formed by more than two layers of bricks.
11. The titanium and titanium alloy melting crucible according to claim 1, wherein the outer shell (1) is a shell which is matched with the boron nitride lining (2) in shape and has the functions of heat insulation, heat preservation and force bearing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200620053250 CN2856899Y (en) | 2006-01-04 | 2006-01-04 | Melting crucible of Ti and Ti alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200620053250 CN2856899Y (en) | 2006-01-04 | 2006-01-04 | Melting crucible of Ti and Ti alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2856899Y true CN2856899Y (en) | 2007-01-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200620053250 Expired - Lifetime CN2856899Y (en) | 2006-01-04 | 2006-01-04 | Melting crucible of Ti and Ti alloy |
Country Status (1)
| Country | Link |
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| CN (1) | CN2856899Y (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100416205C (en) * | 2006-01-04 | 2008-09-03 | 刘宏葆 | Titanium and titanium alloy melting kettle |
| CN105258987A (en) * | 2014-07-08 | 2016-01-20 | 帕纳科有限公司 | Preparation of samples for XRF using flux and platinum crucible |
-
2006
- 2006-01-04 CN CN 200620053250 patent/CN2856899Y/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100416205C (en) * | 2006-01-04 | 2008-09-03 | 刘宏葆 | Titanium and titanium alloy melting kettle |
| CN105258987A (en) * | 2014-07-08 | 2016-01-20 | 帕纳科有限公司 | Preparation of samples for XRF using flux and platinum crucible |
| CN105258987B (en) * | 2014-07-08 | 2020-01-21 | 马尔文帕纳科公司 | Preparation of samples for XRF using flux and platinum crucible |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Effective date of abandoning: 20080903 |
|
| C25 | Abandonment of patent right or utility model to avoid double patenting |