CN100416205C - Titanium and titanium alloy melting kettle - Google Patents
Titanium and titanium alloy melting kettle Download PDFInfo
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- CN100416205C CN100416205C CNB2006100326336A CN200610032633A CN100416205C CN 100416205 C CN100416205 C CN 100416205C CN B2006100326336 A CNB2006100326336 A CN B2006100326336A CN 200610032633 A CN200610032633 A CN 200610032633A CN 100416205 C CN100416205 C CN 100416205C
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Abstract
The invention relates to a titanium and titanium alloy melting crucible, comprising shell, boron nitride lining and barrier layer. The shell covers the boron nitride lining and the barrier layer is attached with the inner surface where the boron nitride lining is contacted with titanium and titanium alloy liquid. The crucible in invention can not react with the titanium. It is provided with not bonding, good flow performance of melting pool, big cubage, low cost, easy maintenance and long service. Especially because the barrier layer exists, boron and nitride enhancement is decreased. The content of boron or nitride in melted titanium and titanium alloy is controlled to less than 100ppm. The quality of titanium alloy is improved effectively.
Description
Technical field
The invention belongs to the Metal Melting crucible, particularly relate to the titanium or titanium alloy melting kettle.
Background technology
Because the fusing point of titanium is high and chemical property is very active; during melting; liquid titanium almost can all react with refractory material such as zirconia, magnesia, silica and aluminium oxide with all crucibles; therefore, cause its melting can not adopt the crucible of conventional refractory material manufacturing to carry out vacuum induction melting.Vacuum consumable electrode electric arc skull melting and the cooling of Forced water cooling copper crucible are often adopted in present industrial titanium or titanium alloy melting.Earlier on copper mould wall, solidify skim " scull " during the vacuum arc skull melting, play protection titanium liquid and do not polluted and heat-blocking action, so that in crucible, form a molten bath by crucible material.Make titanium liquid temp field inhomogeneous because water jacketed copper crucible cools off very fast and forms scull, add that titanium alloy is short in the liquid retention time, feasible cast back titanium alloy casting uneven components.Uneven components is very big to the performance impact of alloy, and is very sensitive to composition as the transformation temperature of Ti-Ni marmem.Specific energy consumption is big mutually with vacuum induction melting for the vacuum arc skull melting, and the smelting titanium alloy power consumption is 40～60kw/kg.For addressing the above problem, the someone proposes to make the titanium or titanium alloy melting kettle with calcium oxide.But calcium oxide is difficult to sinter molding, and lime crucible is easy to hydrolysis under air, and oxygen content can increase in the titanium alloy of this external application lime crucible melting, influences the performance of titanium alloy.The inventor discloses a kind of titanium or titanium alloy melting kettle material and has reached the manufacture method of being made crucible by this material in Chinese patent ZL200410025119.0, adopting boron nitride and an amount of flux is raw material, by be pressed into the crucible blank through isostatic cool pressing, 1800 ℃ of following sintering 1 hour, get final product the melting kettle finished product, and on laboratory scale is used, obtained good effect, have under the high temperature and titanium does not react, not with alloy bonding; Energy consumption is low, the alloying component behind the smelting and pouring is even, the advantage of stable performance.But the technology of above-mentioned patent disclosure, owing to adopt boron nitride to add the technical scheme of the whole crucible of manufacturing of an amount of flux thermal sintering behind the isostatic cool pressing base, can't satisfy industrial production requirement, because the required melting kettle volume of industrialized production is big, adopt the technology of patent ZL200410025119.0 to be difficult to manufacture, its reason is: (1), suitability for industrialized production use crucible (generally being unit with ton) volume big, equipment such as required isostatic cool pressing that boron nitride crucible is whole when making, sintering require high price expensive, and equipment will be made especially.(2), boron nitride crucible made in one piece is too expensive, in case damage and can't repair, must integral replacing, financial cost is uneconomical.(3), easily crack in boron nitride crucible manufacturing made in one piece and the use.
In addition, Zhao Fengming etc. discloses the Preliminary Applications effect of a kind of pyrolytic boron nitride crucible in the titanium or titanium alloy melting and a kind of manufacture method of pyrolytic boron nitride crucible in document " application of pyrolytic boron nitride crucible in extraordinary melting " and " growth of pyrolytic boron nitride crucible material and performance " 2 pieces of papers.Pyrolytic boron nitride (PBN) crucible has many particular performances, as: the pyrolytic boron nitride crucible has the stability of fabulous chemistry and heat, 3000 ℃ of distillations, and its intensity improves with the rising of temperature, and when temperature was 2200 ℃, intensity reached maximum; Acid and alkali resistance at room temperature, salt and organic reagent are convenient to store, and be at high temperature acidproof; Pyrolytic boron nitride crucible density height, pore-free, its density is near the solid density (2.27g/cm of material
3), the metal of molten condition be difficult to infiltrate in the sidewall of crucible, when with monkey melting titanium or titanium alloy, even also very easily pours out in the situation that cools to room temperature with the furnace, and the crucible inwall is bright and clean, does not have the bonding phenomenon, does not stay residue, and crucible cleans easily, can use repeatedly; Compare with the boron nitride crucible of thermal sintering after the process isostatic cool pressing, the pyrolytic boron nitride crucible is at mechanics, aspect of performance such as calorifics and electricity has tangible anisotropy, also have microwave and ultrared superperformance simultaneously, differ about 20 times at deposition direction with perpendicular to the thermal conductivity on the depositional plane direction, that is to say that crucible surface is the good conductor of heat, and be insulator perpendicular to the crucible surface direction, when with this crucible for smelting titanium, the inner thermal field of crucible is even, and heat is difficult to shed by sidewall of crucible, so improved heat-insulating property, can save electric power nearly 1/2nd; The thermal shock resistance of PBN crucible is good in addition, does not directly see crackle in the input water for 2000 ℃.
The same with the disclosed technology of Chinese patent ZL200410025119.0, Zhao Fengming etc. disclose a kind of pyrolytic boron nitride crucible in document " application of pyrolytic boron nitride crucible in extraordinary melting " and " growth of pyrolytic boron nitride crucible material and performance " be boron nitride crucible made in one piece, only be suitable for laboratory and small lot batch manufacture, in industrial-scale production, all have the boron nitride crucible made in one piece three big shortcomings of touching upon previously; No matter be to adopt pyrolytic boron nitride or adopt the melting kettle of sintered boron nitride simultaneously as titanium or titanium alloy, in the titanium or titanium alloy of melting, all there is nitrogen pick-up in varying degrees and increasing the boron phenomenon, nitrogen, boron too high levels can cause fragility in the titanium or titanium alloy, influence alloy property, main dependence adds high-power in actual production at present, shorten smelting time and control nitrogen content and boron content, thereby need improve existing technology, propose new technical scheme, improve the shortcoming of prior art.
Summary of the invention
The object of the present invention is to provide a kind of titanium or titanium alloy melting kettle, can satisfy industrialization, big volume, low cost, easy-maintaining, long requirement of life-span, and the nitrogen pick-up in the alloy and increase the boron phenomenon can effectively reduce the titanium or titanium alloy melting time.
A kind of titanium or titanium alloy melting kettle, described crucible comprises shell, boron nitride liner and barrier layer, and shell coats the boron nitride liner, and the barrier layer is attached to boron nitride liner and the contacted inner surface of titanium or titanium alloy liquid.
---described barrier layer is meant carries out the seasoned conversion zone that contains compound between compound between titanium and the boron or titanium and the nitrogen of handling that the back forms between titanium and the boron nitride.
---described barrier layer is to contain high-melting-point material TiB
2Or the reaction barrier layers of TiB.
---described barrier layer be with boron nitride contain liner be embedded in after the high temperature counterdiffusion, form in titanium powder or titanium powder and the catalyst mix powder contain high-melting-point material TiB
2Or the reaction barrier layers of TiB.
---described barrier layer be boron nitride is contained the mixed coating of liner spray metal titanium or Titanium and catalyst after form after the high temperature counterdiffusion contain high-melting-point material TiB
2Or the reaction barrier layers of TiB.
---the thickness on described barrier layer is between 0.05mm～0.5mm, and preferred thickness is 0.15～0.35mm.
---described boron nitride liner is integral sintered boron nitride liner or pyrolytic boron nitride liner made in one piece.
---described boron nitride liner is cup-shaped structure or the cup-shaped structure of double-deck brick formation or the cup-shaped structure that two-layer above brick forms that forms with the individual layer brick that the sintered boron nitride brick is piled into.
---described boron nitride liner is cup-shaped structure or the cup-shaped structure of double-deck brick formation or the cup-shaped structure that two-layer above brick forms that forms with the individual layer brick that the pyrolytic boron nitride brick is piled into.
---described boron nitride liner is cup-shaped structure or the cup-shaped structure of double-deck brick formation or the cup-shaped structure that two-layer above brick forms that forms with the individual layer brick that the boron nitride monocrystal brick is piled into.
---described shell is meant the housing with thermal insulation, insulation, load function that is complementary with boron nitride liner shape.
The invention has the advantages that:
By seasoned processing, formed the conversion zone, particularly TiB of layer thickness compound between the titaniferous of 0.05mm～0.50mm and the compound between the boron or titanium and nitrogen at boron nitride liner and the contacted inner surface of titanium or titanium alloy liquid
2-TiB conversion zone can stop effectively that boron and nitrogen spread in titanium or titanium alloy liquid, effectively reduced to increase boron and nitrogen pick-up phenomenon when utilizing boron nitride crucible melting titanium or titanium alloy, has improved the quality of titanium or titanium alloy.
Description of drawings
Fig. 1 is the structural representation of the present invention's crucible.
Fig. 2 is the A-A cutaway view of Fig. 1.
The structural representation of the present invention's that Fig. 3 is piled into double-deck boron nitride brick for liner crucible.
The structural representation of the present invention's that Fig. 4 is piled into three layers of boron nitride brick for liner crucible.
Fig. 5 is the structural representation of the present invention's of the boron nitride liner of the integral sintered method manufacturing of employing crucible.
Fig. 6 is the structural representation of the present invention's of employing pyrolytic boron nitride liner made in one piece crucible.
Among the above-mentioned figure: 1 is housing, and 2 is the boron nitride liner, 3 barrier layers.
The specific embodiment
1.1 the manufacturing of sintered boron nitride brick
With boron nitride powder, perhaps boron nitride powder and an amount of flux are mixed, in mould, make brick shape blank through isostatic cool pressing, at 1800 ℃ of following sintering 1-2 hours, can obtain the sintered boron nitride brick.
The flux that uses during the sintered boron nitride brick adopts zirconia, magnesia, boron oxide respectively, as percentage by weight 0.5% zirconia, 1% magnesia and 1.5% boron oxide, can be used as the flux of sintered boron nitride brick.
1.2 the manufacturing of integral sintered boron nitride liner
Its basic technology is identical with the manufacturing process of 1.1 sintered boron nitride bricks, the mould difference that adopts when different is the isostatic cool pressing base, and directly integral body is pressed into required cup-shaped of crucible, then sinter molding at high temperature.
1.3 the manufacturing of pyrolytic boron nitride brick
Adopt the blank of the pyrolytic boron nitride brick of chemical vapor deposition method manufacturing, be machined to required shape and size then, can obtain the pyrolytic boron nitride brick, specific as follows:
With high-purity unstrpped gas BCl
3And NH
3, it is indoor that mixing feeds pyroreaction according to a certain percentage, and the temperature of reative cell is up to 2000 ℃, and mist is undertaken by following chemical reaction equation in reative cell:
BCl
3+NH
3＝BN+3HCl
In the growth course of pyrolytic boron nitride (PBN) material, people always get used to it is likened to snow, the little snowflake of hexagon BN of growth in promptly reacting, constantly heap drops on the graphite matrix (core) of heating, prolongation along with the time, accumulation horizon has promptly formed the housing of pyrolytic boron nitride in thickening, the demoulding take off promptly be independently, pure pyrolytic boron nitride blank.Pyrolytic boron nitride has good machinability, and the pyrolytic boron nitride blank is processed into the shape and size of drawing requirement, has promptly obtained pyrolytic boron nitride brick required for the present invention.
The chemical vapor deposition of pyrolytic boron nitride material not only simply but also complicated.Equipment is simple, and principle is simple, and is simple to operate; But the influence factor complexity of technology, for example, the putting position of the size of the intake method of raw material, charging mode, burner hearth, geometry, core and mode or the like all will exert an influence to gas deposition, also can cause scrapping of whole stove when serious.But gas deposition main influences temperature, the pressure in the stove and the flow-rate ratio of gas that parameter still is a matrix.Generally select 1800～1900 ℃ of temperature for use, furnace pressure 1～2mmHg, the flow of gas will be decided on the size of furnace space, sedimental requirement, for the pyrolytic boron nitride brick that the growth crucible liner is used, selects high-temperature technology usually for use.
The boron nitride brick can have different geometries, particularly can be designed to the shape that can locate mutually of concavo-convex cooperation, not only can conveniently be piled into liner, and is convenient to change after the damage of boron nitride brick.
1.4 the manufacturing of whole pyrolytic boron nitride liner
Its basic technology is identical with the manufacturing process of 1.3 pyrolytic boron nitride bricks, and the different graphite jig differences that adopt when being chemical vapour deposition (CVD) directly adopt the graphite punch, form the required cup-shaped pyrolytic boron nitride liner of crucible.
1.5 the manufacturing of shell
Housing can adopt refractory material (as graphite, calcium oxide, zirconia etc.) manufacturing, reaches the function of thermal insulation, insulation, load, and its shape should be complementary with boron nitride.The most frequently used shell is to adopt graphite to make.
1.6 the formation process implementing example 1 on barrier layer
Be embedded in integral sintered boron nitride liner or whole pyrolytic boron nitride liner in the Titanium powder below-100 orders or in the Titanium powder and catalyst below-100 orders,, can shorten the reaction time as selecting boride as catalyst.Between 1000 ℃～1600 ℃, carried out sintering 2～30 hours,, on the boron nitride liner, can form with TiB by counterdiffusion
2For main body or TiB
2-TiB is dystectic reaction barrier layers of main body, with titanium liquid prepurging 1～2 time, promptly can obtain the TiB of the about 0.05mm～0.5mm of thickness
2The reaction barrier layers of-TiB, preferred thickness are 0.15～0.35mm.
For the boron nitride liner that adopts the boron nitride brick to pile up, no matter be to adopt sintered boron nitride brick or pyrolytic boron nitride brick, the boron nitride liner of in the graphite shell, the boron nitride brick being piled up earlier by design drawing, in the liner of piling up with the boron nitride brick, be filled with in the Titanium powder below-100 orders then or Titanium powder and catalyst below-100 orders, between 1000 ℃～1600 ℃, carried out sintering 2～30 hours, by counterdiffusion, on the boron nitride liner, can form with TiB
2For main body or TiB
2-TiB is dystectic reaction barrier layers of main body, with titanium liquid prepurging 1～3 time, promptly can obtain the TiB of the about 0.05mm～0.5mm of thickness
2The reaction barrier layers of-TiB, preferred thickness are 0.15～0.35mm.
1.7 the formation process implementing example 2 on barrier layer
It no matter is the liner of piling up for whole boron nitride liner or boron nitride brick, the inner surface spraying layer of metal titanium that adopts plasma spraying technology to contact with titanium or titanium alloy liquid at liner, the perhaps mixed coating of Titanium and catalyst, between 1000 ℃～1600 ℃, carrying out sintering 2～30 hours then, by counterdiffusion, on the boron nitride liner, can form with TiB
2For main body or TiB
2-TiB is dystectic reaction barrier layers of main body, with titanium liquid prepurging 1～3 time, promptly can obtain the TiB of the about 0.05mm～0.5mm of thickness
2The reaction barrier layers of-TiB, preferred thickness are 0.15～0.35mm.
1.8 the manufacturing of a titanium or titanium alloy melting kettle
To have the boron nitride liner on barrier layer, be assembled in the shell, promptly obtain a kind of titanium or titanium alloy melting kettle of the present invention by the crucible Design Requirement Drawing.
Can decide according to the composition of the titanium alloy of the size of actual crucible, capacity, main melting and adopt individual layer or bilayer or nitride multilayer boron liner, the thickness on barrier layer and the use material and the support strength of shell.
1.9 the application of a titanium or titanium alloy melting kettle
The present invention's crucible installed to place vaccum sensitive stove smelting titanium alloy, its average power consumption be 2-3kw/kg.The liner of crucible does not at high temperature react with titanium during melting, not with alloy bonding, the molten bath good fluidity, alloying component behind the smelting and pouring is even, stable performance particularly owing to the existence on barrier layer, has effectively reduced and has increased boron and nitrogen pick-up, the boron content of the titanium or titanium alloy after the melting or nitrogen content can be controlled at below the 100ppm, have effectively improved the quality of titanium alloy.
Should be noted that herein openly can replace with the identical structure of other effect that the embodiment that the present invention introduced simultaneously realizes unique structure of the present invention with the structure of explanation.Though preferential embodiment of the present invention is introduced in this article and is illustrated; but those skilled in the art know and know that these embodiment illustrate; those skilled in the art can make countless variations, improvement and replacement; and can not break away from the present invention; therefore, should not limit protection scope of the present invention according to the content and the spirit of literature record of the present invention.
Claims (12)
1. titanium or titanium alloy melting kettle, it is characterized in that, described crucible comprises shell (1), boron nitride liner (2) and barrier layer (3), and shell (1) coats boron nitride liner (2), and barrier layer (3) are attached to boron nitride liner (2) and the contacted inner surface of titanium or titanium alloy liquid.
2. a kind of titanium or titanium alloy melting kettle according to claim 1, it is characterized in that described barrier layer (3) are meant and carry out the seasoned conversion zone that contains compound between compound between titanium and the boron or titanium and the nitrogen of handling that the back forms between titanium and the boron nitride.
3. a kind of titanium or titanium alloy melting kettle according to claim 1 and 2 is characterized in that, described barrier layer (3) are to contain high-melting-point material TiB
2Or the reaction barrier layers of TiB.
4. a kind of titanium or titanium alloy melting kettle according to claim 1, it is characterized in that, described barrier layer (3) be with the boron nitride liner be embedded in after the high temperature counterdiffusion, form in titanium powder or titanium powder and the catalyst mix powder contain high-melting-point material TiB
2Or the reaction barrier layers of TiB.
5. a kind of titanium or titanium alloy melting kettle according to claim 1, it is characterized in that, described barrier layer (3) be with the mixed coating of boron nitride liner spray metal titanium or Titanium and catalyst after form after the high temperature counterdiffusion contain high-melting-point material TiB
2Or the reaction barrier layers of TiB.
6. a kind of titanium or titanium alloy melting kettle according to claim 1 and 2 is characterized in that the thickness of described barrier layer (3) is between 0.05mm～0.5mm.
7. a kind of titanium or titanium alloy melting kettle according to claim 6 is characterized in that the thickness of described barrier layer (3) is 0.15～0.35mm.
8. a kind of titanium or titanium alloy melting kettle according to claim 1 is characterized in that, described boron nitride liner (2) is integral sintered boron nitride liner or pyrolytic boron nitride liner made in one piece.
9. a kind of titanium or titanium alloy melting kettle according to claim 1, it is characterized in that described boron nitride liner (2) is cup-shaped structure or the cup-shaped structure of double-deck brick formation or the cup-shaped structure that two-layer above brick forms that forms with the individual layer brick that the sintered boron nitride brick is piled into.
10. a kind of titanium or titanium alloy melting kettle according to claim 1, it is characterized in that described boron nitride liner (2) is cup-shaped structure or the cup-shaped structure of double-deck brick formation or the cup-shaped structure that two-layer above brick forms that forms with the individual layer brick that the pyrolytic boron nitride brick is piled into.
11. a kind of titanium or titanium alloy melting kettle according to claim 1, it is characterized in that described boron nitride liner (2) is cup-shaped structure or the cup-shaped structure of double-deck brick formation or the cup-shaped structure that two-layer above brick forms that forms with the individual layer brick that the boron nitride monocrystal brick is piled into.
12. a kind of titanium or titanium alloy melting kettle according to claim 1 is characterized in that, described shell (1) is meant the housing with thermal insulation, insulation, load function that is complementary with boron nitride liner (2) shape.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100326336A CN100416205C (en) | 2006-01-04 | 2006-01-04 | Titanium and titanium alloy melting kettle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100326336A CN100416205C (en) | 2006-01-04 | 2006-01-04 | Titanium and titanium alloy melting kettle |
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| Publication Number | Publication Date |
|---|---|
| CN1995885A CN1995885A (en) | 2007-07-11 |
| CN100416205C true CN100416205C (en) | 2008-09-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102980397A (en) * | 2011-09-05 | 2013-03-20 | 鞍钢集团工程技术有限公司 | Graphite crucible |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586891B (en) * | 2012-02-28 | 2015-09-30 | 浙江上城科技有限公司 | A kind of lining combined type high-temperature resisting crucible |
| CN104233196B (en) * | 2014-09-01 | 2017-04-19 | 京东方科技集团股份有限公司 | Evaporation crucible and evaporation device |
| CN108588465B (en) * | 2018-05-15 | 2020-11-06 | 北京交通大学 | Crucible body for preparing particle-reinforced metal-based composite material by stirring method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3734480A (en) * | 1972-02-08 | 1973-05-22 | Us Navy | Lamellar crucible for induction melting titanium |
| US5075055A (en) * | 1990-06-06 | 1991-12-24 | Union Carbide Coatings Service Technology Corporation | Process for producing a boron nitride crucible |
| US5674317A (en) * | 1992-07-02 | 1997-10-07 | Shin-Etsu Chemical Co., Ltd. | Vessel made from pyrolytic boron nitride |
| CN1583670A (en) * | 2004-06-11 | 2005-02-23 | 上海大学 | Titanium and titanium alloy smelting furnace materials |
| CN1699906A (en) * | 2005-05-26 | 2005-11-23 | 周星 | Composite crucible for smelting titanium and titanium alloy |
| CN2856899Y (en) * | 2006-01-04 | 2007-01-10 | 刘宏葆 | Melting crucible of Ti and Ti alloy |
-
2006
- 2006-01-04 CN CNB2006100326336A patent/CN100416205C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3734480A (en) * | 1972-02-08 | 1973-05-22 | Us Navy | Lamellar crucible for induction melting titanium |
| US5075055A (en) * | 1990-06-06 | 1991-12-24 | Union Carbide Coatings Service Technology Corporation | Process for producing a boron nitride crucible |
| US5674317A (en) * | 1992-07-02 | 1997-10-07 | Shin-Etsu Chemical Co., Ltd. | Vessel made from pyrolytic boron nitride |
| CN1583670A (en) * | 2004-06-11 | 2005-02-23 | 上海大学 | Titanium and titanium alloy smelting furnace materials |
| CN1699906A (en) * | 2005-05-26 | 2005-11-23 | 周星 | Composite crucible for smelting titanium and titanium alloy |
| CN2856899Y (en) * | 2006-01-04 | 2007-01-10 | 刘宏葆 | Melting crucible of Ti and Ti alloy |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102980397A (en) * | 2011-09-05 | 2013-03-20 | 鞍钢集团工程技术有限公司 | Graphite crucible |
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| CN1995885A (en) | 2007-07-11 |
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