CN1633511A - High-purity spongy titanium material and its production method - Google Patents
High-purity spongy titanium material and its production method Download PDFInfo
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- CN1633511A CN1633511A CN02827453.9A CN02827453A CN1633511A CN 1633511 A CN1633511 A CN 1633511A CN 02827453 A CN02827453 A CN 02827453A CN 1633511 A CN1633511 A CN 1633511A
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- vacuum separation
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1295—Refining, melting, remelting, working up of titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
- C22B34/1268—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams
- C22B34/1272—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/14—Refining in the solid state
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- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Physical Vapour Deposition (AREA)
Abstract
A high-purity spongy titanium material containing less amounts of oxygen and metal elements is economically produced. The vacuum separation time t in a vacuum separation step is t = tO + 15 to + 35 hour where tO is the time from the start of the vacuum separation till the time when the temperature of the central part of the material in a reaction vessel reaches to a stable temperature. At and near the central part of the material where the amounts of metal elements are a little, the specific area measured by the BET method is below 0.05 m2/g. The amount of oxygen after cutting and crushing is suppressed to a low level even if the cutting and crushing are carried out in the atmosphere.
Description
Technical field
The present invention relates to a kind of raw-material high purity titanium sponge material and manufacture method thereof that is suitable as spraying plating with target.
Background technology
As the industrially preparing process of metal titanium, what mostly use is the titanium sponge material cutting and grinding that will make with Kroll process, forms piece then, and the method that its dissolving is cast.Kroll process is made up of following two operations: the reduction operation that makes fusion Mg and titanium tetrachloride reaction in reaction vessel; The vacuum separation operation of removing by in this reaction vessel, heating, make unreacted Mg in the material that is included in the container and the evaporation of residual by product with reduction back with vacuum state.
On the other hand, as the new purposes of metal titanium, can enumerate the wiring material in semiconductor elements such as LSI.This distribution is by being that target carries out spraying plating and forms with highly purified metal titanium., for target, require impurity wherein few, and, require its oxygen level below 200ppm, and the content of Fe, Ni, Cr, Al and each metallic element of Si is below 10ppm for this spraying plating as its raw-material titanium sponge material.
But, because Kroll process is to be preferential method with production efficiency, so be not easy to guarantee in spraying plating with desired impurity level in the target.Therefore, following method has been proposed.One is after vacuum separation, near the center system of selection (speciallyying permit communique No. 2863469) of the portioned productization center that will remove top, bottom and the peripheral portion of the titanium sponge material that obtains and obtain in reaction vessel, another is the low humidity breaking method (speciallyying permit communique No. 2921790) of the titanium sponge material cutting and grinding in the atmosphere of low humidity that will be taken out by this reaction vessel.
Yet, in the former center system of selection, though can guarantee for oxygen, to be difficult to guarantee this level in spraying plating desired level in the target for each metallic element of Fe, Ni, Cr, Al and Si.In contrast, in the latter's low humidity breaking method,, can guarantee in spraying plating desired level in the target, and for each metallic element of Fe, Ni, Cr, Al and Si, be difficult to guarantee this level for oxygen.
Therefore, if will make each metallic element of Fe, Ni, Cr, Al and Si and this two aspect of oxygen all guarantee to be used in combination the former center system of selection and the latter's low humidity breaking method in spraying plating desired level in the target.But, in fact the problem of Cun Zaiing is, the former center system of selection is implemented easily, and under the situation of the latter's low humidity breaking method, if in fact want stably to guarantee spraying plating desired oxygen level in the target, then need inside is remained the very large isolated operating space of low humidity,, can not be referred to as practical method owing to construct with atmosphere to keep needing much more very funds at this spatial.
Summary of the invention
The object of the present invention is to provide oxygen amount and metallic element amount the two high purity titanium sponge material and manufacture method thereof all less and economical.
In order to achieve the above object, the inventor has studied the sampling location of the titanium sponge material made from Kroll process and the relation between the oxygen amount emphatically.
Fig. 1 is the longitudinal sectional drawing of the titanium sponge material in the reaction vessel in the vacuum separation operation.Reaction vessel 20 is housed in the process furnace 30.Owing in above-mentioned reduction operation, can separate out titanium with the side wall inner surfaces of reaction vessel 20 on the fire grate 21 in reaction vessel 20, so the titanium sponge materials 10 in the reaction vessel 20 become the thinner shape of stage casing part.
In the titanium sponge material 10 after the vacuum separation operation, more away from top, following and peripheral surface part, each metal element content of Fe, Ni, Cr, Al and Si is few more.This is because each metallic element that contains is mainly produced by the pollution of reaction vessel 20.Therefore,, choose near the part 11 remaining center,, can guarantee spraying plating desired level in the target more easily for metallic element by top, bottom and the peripheral portion that removes titanium sponge material 10.
But, beat all be the oxygen amount particularly the oxygen amount after the cutting and grinding reduce to some extent in the top layer of titanium sponge material 10 part.For example, if to distributing, then many more near 1/2 portion C oxygen amount more in the oxygen amount after the part of topmost portion A to the 1/2 portion C investigation cutting and grinding on the central position of titanium sponge material 10.When the titanium particulate oxygen amount that obtains from topmost portion A is 250ppm, being about 300ppm at 1/4 part B for example, is about 350ppm in 1/2 portion C.Because the existence of this trend, even choose near the part 11 in the center of titanium sponge material 10, the oxygen amount after the cutting and grinding also is difficult to guarantee spraying plating desired level in the target.
The inventor from rerum natura and method for making two aspects to investigating in the top layer of the titanium sponge material 10 few reason of partial oxygen quantitative change.The following fact that this result is clear and definite.
Fig. 2 is topmost portion A, the 1/4 part B for the central position, the figure that 1/2 portion C is represented the temperature variation of the titanium sponge material in the vacuum separation operation.The variation of temperature trend of any part all is that the vacuum separation operation begins the temporary transient decline in back, changes rising then into, reaches the equilibrium temperature near furnace temperature.This is because of residual Mg in the beginning vacuum separation also start vaporizer, and because of this vaporization heat, temperature can temporarily descend, and still the minimizing temperature along with residual Mg can rise gradually, and when evaporation finishes, temperature will be stabilized in the level near furnace temperature.
The arbitrary part of this trend in topmost portion A, 1/4 part B, 1/2 portion C is all identical, but minimum temperature descends according to the order of topmost portion A, 1/4 part B, 1/2 portion C, from the beginning vacuum separation to the time that begins to change into rising, time of reaching equilibrium temperature is elongated according to the order of topmost portion A, 1/4 part B, 1/2 portion C.This is because be difficult to more break away near the residual Mg of the centre portions of titanium sponge material more, is made as moment of vacuum separation end with removing centre portions that this residual Mg is difficult to break away from most, moment that promptly the temperature T c of this part reaches equilibrium temperature To behind the residual Mg of 1/2 portion C.Also have, why to reduce according to the order of topmost portion A, 1/4 part B, 1/2 portion C be because remarkable to the heat release of opening portion one side (top) of reaction vessel to equilibrium temperature.
The result who carries out vacuum separation with this technology is, in the top layer part away from titanium sponge material center, heated condition that also can be for a long time after the evaporation of Mg finishes becomes the so-called empty state that burns.The inventor thinks that the heat-up time after this Mg evaporation is relevant with the oxygen amount after the cutting and grinding, therefore various investigation have been carried out, found that more centre portions away from the titanium sponge material, pining for sintering in adding of this sky burning state can obtain promoting, make specific surface area become more little, and the more little increase that can be suppressed at the oxygen amount that produces by oxidation in the cutting and grinding operation more of specific surface area, its result, oxygen amount after the cutting and grinding will be according to 1/2 portion C, 1/4 part B, the order of topmost portion A tails off, if after the evaporation of the Mg of 1/2 portion C finishes, also continue heating, then sintering can take place in this part, causes specific surface area to diminish, thereby can realize suboxide.
The present invention is found to be the basis with this and finishes, and this high purity titanium sponge material is the titanium sponge material made from Kroll process, wherein will be defined as 0.05m with the specific surface area that the BET method is measured
2Below/the g, and each metal element content of Fe, Ni, Cr, Al and Si is defined as below the 10ppm.
By the specific surface area of measuring with the BET method is restricted to 0.05m
2Below/the g, even carry out cutting and grinding in common air atmosphere, this titanium particulate oxygen level also can suppress for below the 300ppm.Be preferably 0.04m
2Below/the g, 0.03m more preferably
2Below/the g, further reduce oxygen level thus.Oxygen level after the preferred cutting and grinding is below the 200ppm, more preferably below the 100ppm.For the lower limit of specific surface area, low more good more from reducing the viewpoint of oxygen amount, if but specific surface area is too small, and then the cutting and grinding meeting becomes difficult, so be preferably 0.01m
2More than/the g.
Why each metal element content of Fe, Ni, Cr, Al and Si being defined as below the 10ppm is top, bottom and peripheral portion in order to get rid of the titanium sponge material.Be subjected to the influence of the heating of empty burning state, the specific surface area with the measurement of BET method of these top layer parts, example topmost portion A as shown in FIG. 1 is less.But each metal element content has surpassed 10ppm in this part.The content of preferred especially each metallic element is below the 7ppm.
In addition, the manufacture method of high purity titanium sponge material of the present invention is a method as described below, promptly, when making the titanium sponge material with Kroll process, the time rule that the central part temperature T c that begins the material in the reaction vessel from vacuum separation is reached near the equilibrium temperature To the furnace temperature is to hour, vacuum separation time t in the vacuum separation operation is set at t=to+ (15～35) hour, and after vacuum separation finishes, with near the portioned productization center of removing top, bottom and peripheral portion of the material in the reaction vessel.
By vacuum separation time t being set at more than (to+15) hour, the specific surface area of part can diminish near the center of removing top, bottom and peripheral portion of the material in the reaction vessel, thereby can realize the suboxide after the cutting and grinding.Then, by with near the portioned productization center of removing top, bottom and peripheral portion of the material in the reaction vessel,, also its content can be suppressed on the lower level even for each metallic element of Fe, Ni, Cr, Al and Si.
If vacuum separation time t surpasses (to+35) hour, then specific surface area can become too small, is difficult to carry out cutting and grinding.In addition, thermal equilibrium can deteriorate into more than the necessary degree.More than following being limited to (to+20) of particularly preferred vacuum separation time t hour, for the upper limit for below (to+30) hour.
Also have, in the operation of reality, the central part temperature of not actual measurement titanium sponge material.In each operating equipment, utilize and resolve the temperature variation data that obtain by test operation and temperature and obtain the central part temperature and reach the required time of equilibrium temperature, and be that benchmark is set the heat-up time in the vacuum separation operation with this time.
Description of drawings
Fig. 1 is the longitudinal sectional drawing of the titanium sponge material in the reaction vessel in the vacuum separation operation, Fig. 2 is the figure that topmost portion A, 1/4 part B, 1/2 portion C to the central position is illustrated in the titanium sponge material temperature variation in time in the vacuum separation operation, Fig. 3 is that the diameter (retort diameter) with reaction vessel is illustrated in the vacuum separation operation graphic representation of preferred vacuum separation time as parameter, and Fig. 4 is the microphotograph of the sample chosen by the centre portions of two kinds of titanium sponge materials of different vacuum separation time.
Embodiment
Below embodiments of the present invention are described.
By in reaction vessel, making the Mg fusion, and the titanium tetrachloride liquid of dripping, the titanium sponge material made.After this reduction operation finishes, be transferred to the vacuum separation operation.In the vacuum separation operation, by with becoming vacuum state in the reaction vessel, be heated to specified temperature with process furnace simultaneously, remove unreacted Mg and by product.
Test operation example with Fig. 2 explains this vacuum separation operation.The temperature T a of the topmost portion A of the titanium sponge material in the reaction vessel begins that in vacuum separation a little decline is arranged at first, but can change ascendant trend into, begins to reach equilibrium temperature in about 20-30 hour from vacuum separation at once.In contrast, the temperature T c of centre portions (1/2 portion C) begins to descend about 30 hours continuously from vacuum separation, then, changes into and rises and begin to reach equilibrium temperature To after about 70 hours from vacuum separation.
In the past, with central part temperature T c reach equilibrium temperature To required, the about 70 hours end vacuum separation that are as the criterion, and, do not consider specially with its prolongation only aspect shortening this time some trials being arranged.Its result in the part, owing to do not carry out the heating that the sky after the Mg evaporation burns state, does not carry out sintering, so specific surface area can not reduce fully near the few center of metallic element amount.Therefore, after the vacuum separation, even what choose is near the part center, when carrying out cutting and grinding in air atmosphere, the oxygen amount that is caused by oxidation increases and still becomes comparatively obvious, thereby is difficult to realize that spraying plating is with desired suboxide level in the target.
Therefore, in the present embodiment, after central part temperature T c reaches equilibrium temperature To, also continue heating 15-35 hour, preferred 20-30 hour.Therefore, part is also carried out sintering near the few center of metallic element amount, can make the specific surface area of measuring according to the BET method be reduced to 0.05m thus
2Below/the g.Its result increases by choosing near the part center after the vacuum separation, can be suppressed at the oxygen amount that is produced by oxidation in the cutting and grinding operation, for oxygen amount and metallic element amount, can realize that spraying plating is with desired impurity level in the target.
Part chooses near the center after vacuum separation, as shown in Figure 1, the piece height of titanium sponge material 10 is defined as H, piece directly is defined as D, to begin the thickness h counted 1 from above, to begin the thickness h 2 counted be that peripheral portion cutting more than the 0.18D is removed for the top more than the 0.1H, from below for the bottom more than the 0.25H and from the thickness d that peripheral surface begins to count, and chooses near part 11 30% the center of piece weight of not enough titanium sponge material 10 in this remainder.
For near part 11 center of choosing, in air atmosphere, carry out cutting and grinding usually, thereby become the titanium sponge particle of designated size.Though in air atmosphere, carry out cutting and grinding usually, but still the oxygen amount can be suppressed for below the 300ppm, and each metallic element of Fe, Ni, Cr, Al and Si also can suppress for below the 10ppm.Median size after preferred the pulverizing is 10-300mm.
To the results are shown among Fig. 3 of investigating of the preferred vacuum separation time in the vacuum separation operation.The preferred vacuum separation time is the zone of representing with oblique line among Fig. 3.
The vacuum separation time is subjected to the influence of reaction vessel diameter (retort diameter), and the big more time of this diameter becomes long more.With respect to the vacuum separation time of representing with solid line in the past, the vacuum separation time among the present invention is+15 hours～+ 35 hours.More than+15 hours the time, the specific surface area of part becomes 0.05m near the center of measuring with the BET method
2Below/the g, the oxygen quantitative change after the cutting and grinding is below the 300ppm.In addition, more than+20 hours the time, the part specific surface area becomes 0.03m near the center of measuring with the BET method
2Below/the g, the oxygen quantitative change after the cutting and grinding is below the 200ppm.As the not enough 0.01m of the specific surface area of measuring with the BET method
2During/g, be difficult to carry out cutting and grinding.
For the diameter (retort diameter) of reaction vessel, preferred 1350-2000mm.When not enough 1350mm, even choose at the center, metallic impurity also have the trend of increase.When surpassing 2000mm, might produce the problem of the equipment aspects such as thermal distortion of reaction vessel.
Also have, temperature variation shown in Fig. 2 is the situation of diameter (retort diameter) when the 1700mm of reaction vessel, the vacuum separation time in the past is 70 hours, and the vacuum separation time among the present invention at this moment is 85～105 hours, preferred especially 90～100 hours.
The diameter (retort diameter) that has demonstrated reaction vessel with identical ratio of enlargement in (b) at Fig. 4 (a) is under the situation of 1700mm, and the vacuum separation time is the microphotograph of sample of the centre portions that is selected from the titanium sponge material of 70 hours and 95 hours.
The specific surface area of measuring with the BET method is 0.1m when the vacuum separation time is 70 hours
2/ g, and be to become 0.03m under 95 hours the situation in the vacuum separation time
2/ g.This difference also can be found out in (b) by Fig. 4 (a).Because this specific surface area difference, the result cuts under air atmosphere and is ground in stage of particle that median size is 65mm, being that the oxygen amount is 320ppm under 70 hours the situation in the vacuum separation time, is that the oxygen amount is 190ppm under 95 hours the situation in the vacuum separation time.In addition, for the metallic element amount, each metal element content of Fe, Ni, Cr, Al and Si is all below 10ppm under which kind of situation.
Also have, if it is represent the zone that the oblique line among usefulness Fig. 3 shows, then as follows with mathematical expression.
Vacuum separation time=(0.0698 * [retort diameter]-24) ± 10
So-called BET method is the method by the absorbed dose calculated specific surface area of liquid nitrogen, is widely used in usually in the sorbent material etc.
Industrial utilizability
As described above, high-purity spongy titanium material of the present invention will be by being restricted to 0.05m with the specific area that the BET method is measured2Below/the g, even in air atmosphere, carry out cutting and grinding, also can The oxygen amount is suppressed on the reduced levels, and chooses method by the employing center metal impurities are reduced, Can guarantee economically thus simultaneously spraying plating desired impurity level in the target.
In addition, in the manufacture method of high-purity spongy titanium material of the present invention, it is to hour by near the central part temperature T c that begins the material in the reaction vessel from vacuum separation is reached the furnace temperature the required time rule of equilibrium temperature To, vacuum separation time t in the vacuum separation operation is set at t=to+(15～35) hour, can be restricted to easily 0.05m to the specific area of measuring with the BET method2/ g Below, and utilize the minimizing of the oxygen amount of bringing thus and choose the metal impurities that method is brought by the center Minimizing, can guarantee economically that spraying plating is with desired impurity level in the target.
Claims (2)
1. high purity titanium sponge material, it is the titanium sponge material made from Kroll process, the specific surface area of measuring with the BET method is at 0.05m
2Below/the g, and each metal element content of Fe, Ni, Cr, Al and Si is below 10ppm.
2. the manufacture method of a high purity titanium sponge material, wherein, when making the titanium sponge material with Kroll process, near the required time rule of equilibrium temperature To that the central part temperature T c that begins the material in the reaction vessel from vacuum separation is reached the furnace temperature is to hour, vacuum separation time t in the vacuum separation operation is set at t=to+ (15～35) hour, after vacuum separation finishes, near the part center of removing top, bottom and peripheral portion of the material in the reaction vessel is carried out commercialization.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000238487A JP3756047B2 (en) | 2000-08-07 | 2000-08-07 | High purity titanium sponge material and method for producing the same |
| PCT/JP2002/001118 WO2003066914A1 (en) | 2000-08-07 | 2002-02-08 | High-purity spongy titanium material and its production method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1633511A true CN1633511A (en) | 2005-06-29 |
| CN100487144C CN100487144C (en) | 2009-05-13 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB028274539A Expired - Lifetime CN100487144C (en) | 2000-08-07 | 2002-02-08 | High-purity spongy titanium material and its production method |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP3756047B2 (en) |
| CN (1) | CN100487144C (en) |
| AU (1) | AU2002232157A1 (en) |
| EA (1) | EA006077B1 (en) |
| WO (1) | WO2003066914A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948961A (en) * | 2010-10-08 | 2011-01-19 | 洛阳双瑞万基钛业有限公司 | Manufacturing method of magnesium chloride discharge pipe of reactor for producing sponge titanium |
| CN101517103B (en) * | 2006-09-25 | 2011-10-05 | 埃尔温斯·布卢姆伯格斯 | Method and apparatus for continuous producing of metallic titanium and titanium-based alloys |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3756047B2 (en) * | 2000-08-07 | 2006-03-15 | 住友チタニウム株式会社 | High purity titanium sponge material and method for producing the same |
| JP4766931B2 (en) * | 2005-06-16 | 2011-09-07 | Ｎｔｎ株式会社 | Dielectric ceramics and method for manufacturing the same |
| CN100383266C (en) * | 2006-08-11 | 2008-04-23 | 遵义钛业股份有限公司 | Titanium tetrachloride atomization method of preparing titanium sponge using magnesium |
| CN102534261B (en) * | 2012-01-18 | 2013-04-10 | 深圳市新星轻合金材料股份有限公司 | Process method for preparing titanium sponge |
| JP6924120B2 (en) * | 2017-11-02 | 2021-08-25 | 東邦チタニウム株式会社 | Manufacturing method of titanium sponge |
| CN113718104A (en) * | 2021-08-31 | 2021-11-30 | 新星轻合金材料(洛阳)有限公司 | Preparation process of low-oxygen high-titanium-iron alloy |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6160839A (en) * | 1984-08-29 | 1986-03-28 | Hiroshi Ishizuka | Refining method refractory metal |
| JP2915779B2 (en) * | 1994-03-24 | 1999-07-05 | 株式会社住友シチックス尼崎 | Method for producing high purity titanium material for thin film formation |
| JP2001262246A (en) * | 2000-03-17 | 2001-09-26 | Toho Titanium Co Ltd | Method for producing sponge titanium |
| JP3671133B2 (en) * | 2000-03-30 | 2005-07-13 | 東邦チタニウム株式会社 | Method for producing titanium |
| JP3756047B2 (en) * | 2000-08-07 | 2006-03-15 | 住友チタニウム株式会社 | High purity titanium sponge material and method for producing the same |
-
2000
- 2000-08-07 JP JP2000238487A patent/JP3756047B2/en not_active Expired - Lifetime
-
2002
- 2002-02-08 CN CNB028274539A patent/CN100487144C/en not_active Expired - Lifetime
- 2002-02-08 AU AU2002232157A patent/AU2002232157A1/en not_active Abandoned
- 2002-02-08 EA EA200401055A patent/EA006077B1/en not_active IP Right Cessation
- 2002-02-08 WO PCT/JP2002/001118 patent/WO2003066914A1/en active Application Filing
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101517103B (en) * | 2006-09-25 | 2011-10-05 | 埃尔温斯·布卢姆伯格斯 | Method and apparatus for continuous producing of metallic titanium and titanium-based alloys |
| CN101948961A (en) * | 2010-10-08 | 2011-01-19 | 洛阳双瑞万基钛业有限公司 | Manufacturing method of magnesium chloride discharge pipe of reactor for producing sponge titanium |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2003066914A1 (en) | 2003-08-14 |
| JP3756047B2 (en) | 2006-03-15 |
| AU2002232157A1 (en) | 2003-09-02 |
| JP2002053922A (en) | 2002-02-19 |
| EA006077B1 (en) | 2005-08-25 |
| EA200401055A1 (en) | 2004-12-30 |
| CN100487144C (en) | 2009-05-13 |
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