CN102161473A - Vacuum furnace device for sponge titanium hydrogenation and hydrogenation method of sponge titanium - Google Patents
Vacuum furnace device for sponge titanium hydrogenation and hydrogenation method of sponge titanium Download PDFInfo
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- CN102161473A CN102161473A CN 201110057619 CN201110057619A CN102161473A CN 102161473 A CN102161473 A CN 102161473A CN 201110057619 CN201110057619 CN 201110057619 CN 201110057619 A CN201110057619 A CN 201110057619A CN 102161473 A CN102161473 A CN 102161473A
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Abstract
The invention relates to a vacuum furnace device for sponge titanium hydrogenation and a hydrogenation method of sponge titanium, in particular to a device and a method for preparing titanium powder. By the device and the method disclosed by the invention, the problem that the oxygen content of produced titanium powder is too high in the prior art is solved, the hydrogenation time is substantially shortened, and simultaneously the lower oxygen content of the titanium powder is ensured. The device comprises a furnace wall, wherein heating devices are arranged on the inner wall of the furnace wall, and a furnace tank pipe is put in the space defined by the furnace wall from the upper end of the furnace wall; a hanging ring is arranged on a furnace cover which is arranged at the top end of the furnace tank pipe, and a hydrogen filing pipe penetrates through the furnace cover and is inserted into the sponge titanium powder which is arranged inside the furnace tank pipe; and the furnace tank pipe is connected with an external vacuumizing system. In the method for hydrogenating sponge titanium with the vacuum furnace device, under the vacuum condition, hydrogen is introduced to react with titanium powder after temperature and pressure are adjusted, temperature and pressure are continuously adjusted in the whole process, and the temperature is quickly reduced by quickly separating the furnace wall from the furnace tank pipe; therefore, the time is saved, the production cycle is shortened, and the low oxygen content of the titanium powder is effectively controlled. The vacuum furnace device and the hydrogenation method can be applied to the preparation and processing of the sponge titanium.
Description
Technical field
The present invention relates to a kind of device for preparing titanium valve and preparation method thereof, particularly relate to and a kind ofly prepare the vacuum oven of low oxygen content titanium valve and utilize this vacuum oven to carry out titanium valve hydrogenant method.
Technical background
Titanium or titanium alloy has that density is low, specific tenacity is high, erosion resistance is strong, good, the advantages such as welding property is good, biocompatibility excellence of creep-resistant property under the high temperature.But titanium sponge can't directly use, and therefore, is used for the titanium valve that powder metallurgy technology needs the spongy titanium powder deep processing to form.Titanium sponge has very big air-breathing property, and in hydrogenation process, airborne oxygen, nitrogen and the water vapour that can infiltrate with flange and the valve from bell, connecting tube react, and causing fatal harm is exactly that oxygen level increases and the quality of reduction titanium valve.
The huge impellent of titanium industry development is from defence and military demands such as Aeronautics and Astronautics.From the early stage cost of disregarding, many till now ultralights, ultra-thin, complicated precision component, and the premium properties such as high temperature resistant, corrosion-resistant of titanium material make it huge demand.Simultaneously, the degree of dependence of technology is grown with each passing day, powder metallurgy, casting have become the meet the demands main technique means of precision parts of processing.This causes that directly the quality of powdered material is also had new requirement: such as, the low oxygen content high quality powder is the available prerequisite, therefore has important use to be worth and effect in the development of military technique equipment.
When the spongy titanium powder hydrogen treatment, titanium is in inhaling the hydrogen process, and along with the increase of dissolving in the hydrogen amount, the lattice parameter of its matrix increases gradually, and causes the elastic distortion of dot matrix, causes volume to increase.Why the titanium hydride crystal is by cleavage, due to its Strength Changes of all directions connecting forces.Behind titanium and hydrogen generation TiH2, the volume ratio matrix expands 15%, and makes the lattice of matrix that serious torsional deformation take place, and has produced internal stress.When the hydride of separating out when the crystal boundary place forms the successive reticulated structure, produced successive stretching internal stress, this stretching internal stress is far longer than the metal bonding force, and the plasticity of metal is destroyed.Titanium hydride is the fragility phase, is easy to cleavage when being subjected to the external force hammering, even the power of expanding with heat and contract with cold in hydrogenation process also makes its autoclasis pulverize.
So we need reduce oxygen level in the hydrotreated process of titanium, guarantee the quality of titanium valve processing.
Summary of the invention
The purpose of this invention is to provide a kind of vacuum oven device that can effectively prevent titanium sponge oxygen level increase in hydrogenation process, another purpose provides a kind of said apparatus that utilizes and carries out the hydrotreated method of titanium sponge, can significantly shorten hydrogenation time, save production cost, guaranteed the low oxygen content of titanium valve simultaneously.
For achieving the above object, the technical solution used in the present invention is: a kind of titanium sponge hydrogenant vacuum oven device that is used for, the furnace wall that comprises inner hollow and upper end open, the furnace wall inwall is provided with heating unit, the retort pipe is put into from the furnace wall upper end, the vertical bell of retort pipe is provided with hoisting ring, and hydrogen tube passes bell and is inserted in the inner spongy titanium powder of placing of retort pipe, and the retort pipe is connected with outside pumped vacuum systems.
The position that described retort pipe outer wall contacts with the furnace wall upper end open is provided with the thermoscreen that prevents that internal heat is scattered and disappeared, and described hydrogen tube is inserted on the spongy titanium powder wall partly and offers a plurality of equally distributed apertures.
Described heating unit is a plurality of, is distributed in sidewall and bottom in the furnace wall, and each heating unit is connected with a thermopair that is used to monitor its temperature variation and control its power.
A kind ofly utilize above-mentioned vacuum oven device to carry out titanium sponge hydrogenant method, comprise the following steps:
A, spongy titanium powder to be processed is packed in the retort pipe, whether other utility appliance of corresponding inspection is intact, prepares to start start;
B, open outside pumped vacuum systems, in the given time, vacuum tightness reaches 10
-2-10
-3Pa opens heating unit simultaneously, is rapidly heated 270 ℃-320 ℃ the time when thermopair monitors temperature, feeds hydrogen in the retort pipe;
C, hydrogen and spongy titanium powder react, and are heated to 630 ℃-670 ℃ and be incubated 1.5-2.5 hour, and hydrogen pressure remains on 0.15-0.25MPa, begin to be cooled to 280 ℃-320 ℃ subsequently after, end logical hydrogen;
D, when being cooled to 180 ℃-220 ℃, by hoisting ring the retort pipe is hung furnace wall, and the retort pipe is cooled to room temperature, simultaneously, be placed on fully in the refrigerative furnace wall installing the retort pipe for the treatment of the hydrogen treatment spongy titanium powder, carry out the hydrogenation of next batch spongy titanium powder.
From every technical characterictic of the invention described above as can be seen, its advantage is: the present invention adopts energy-efficient vacuum oven pot type device to add electric heater unit, significantly shorten hydrogenation time, effectively prevent the increase of titanium sponge oxygen level in hydrogenation process, the present invention has saved production cost, make full use of the waste heat of furnace wall, shortened the production cycle, had good application and popularization value.
Description of drawings
The present invention will illustrate by way of compared with accompanying drawings and combined with example:
Fig. 1 be vacuum oven device of the present invention the structure cross-sectional schematic;
Fig. 2 is a heating unit distribution schematic diagram of the present invention;
Fig. 3 is a hydrogen tube structural representation of the present invention;
Wherein Reference numeral 1 is that furnace wall 2 is that heating unit 3 is retort pipes
The 4th, bell 5 is that hoisting ring 6 is that hydrogen tube 7 is spongy titanium powders
The 8th, pumped vacuum systems 9 is that thermoscreen 10 is that aperture 11 is thermopairs.
Embodiment
The present invention is described further by embodiment below in conjunction with accompanying drawing:
Preferred embodiment
As shown in Figure 1-Figure 3; vacuum oven device of the present invention is when carrying out spongy titanium powder hydrogenation; vacuumize earlier; when vacuum tightness reaches specified requirement; open heating unit; wherein heating unit is evenly distributed on sidewall and the bottom in the furnace wall; when temperature be rapidly heated 270-320 ℃ (this moment temperature can select as required; such as 270; 275; 280; 285; 290; 295; 300; 305; 310; 315; 320 ℃) time; fill hydrogen by the spongy titanium powder of hydrogen tube in the retort pipe; in order to make the titanium valve hydrogenation process even; we are on the tube wall of the lower end of hydrogen tube; just be inserted into the part of spongy titanium powder; offer a plurality of apertures; hydrogen can be punched in the titanium valve rapidly and uniformly; after hydrogen and titanium valve react; slowly (this moment can as required select to 630-670 ℃ by temperature for Heating temperature; such as 630; 635; 640; 645; 650; 655; 660; 665; 670 ℃) and (time this moment can be selected as required to be incubated 1.5-2.5 hour; such as 1.5; 1.6; 1.8; 1.9; 2.0; 2.2; 2.4; 2.5 hour); the pressure of this process hydrogen remains on 0.15-0.25MPa(pressure this moment and can select as required; such as 0.15; 0.16; 0.18; 0.19; 0.21; 0.23; 0.25 MPa); (this moment, temperature can be selected as required to be cooled to 280-320 ℃ then; such as 280; 285; 290; 295; 300; 305; 310; 315; 320 ℃); end to feed hydrogen again; when temperature is cooled fast to 180-220 ℃; it is very slow that this moment, temperature reduced meeting; if will be reduced to room temperature again; then need for a long time; and the titanium hydride powder in the retort pipe has few part to react because air is infiltrated at the connecting tube place; cause the oxygen nitrogen content of titanium hydride powder to increase; so (this moment, temperature can be selected as required to be reduced to 180-220 ℃ in temperature; such as 180; 185; 190; 195; 200; 205; 210; 215; 220 ℃) time; we hang furnace wall by hoisting ring with the retort pipe; make the temperature of retort pipe be cooled fast to room temperature then; the retort pipe that will install spongy titanium powder simultaneously in addition is placed in the incomplete refrigerative furnace wall; carry out the hydrogenation of next batch spongy titanium powder; whole process has not only shortened cooling time; saved production cost; and made full use of the waste heat of furnace wall, shortened the production cycle.
On to temperature controlling and monitoring, we are provided with thermopair by the rear end at heating unit, to the monitoring temperature of heating unit and the power of control heating unit, and heating unit is set to a plurality of, can make the temperature in the retort pipe more even, make spongy titanium powder that hydrogenation fully take place in the short period of time.
In hydrogenation process of the present invention, need to consider to finish fast in the retort pipe to feed hydrogen, also to consider production safety, therefore, at 270 ℃ of-320 ℃ of beginnings logical hydrogen in the retort pipe, continue slowly to be heated to 630 ℃-670 ℃, beginning heat-insulation pressure keeping: insulation 1.5-2.5 hour, the retort intraductal pressure keeps 0.15-0.25MPa, when being cooled to 280-320 ℃, stops to feed hydrogen again.
Among the present invention, hydrogen is as reactant gases, after the spongy titanium powder reaction, and resulting titanium hydride powder.By visual inspection, find that very significantly crack performance appears in the titanium hydride surface.And fragility increases greatly than titanium sponge, so that pulverize.
Disclosed all features in this specification sheets except mutually exclusive feature, all can make up by any way.
Disclosed arbitrary feature in this specification sheets (comprising any accessory claim, summary and accompanying drawing) is unless special narration all can be replaced by other equivalences or the alternative features with similar purpose.That is, unless special narration, each feature is an example in a series of equivalences or the similar characteristics.
Claims (4)
1. one kind is used for titanium sponge hydrogenant vacuum oven device, it is characterized in that comprising the furnace wall (1) of inner hollow and upper end open, furnace wall (1) inwall is provided with heating unit (2), retort pipe (3) is put into from furnace wall (1) upper end, the vertical bell 4 of retort pipe (3) is provided with hoisting ring (5), hydrogen tube (6) passes bell (4) and is inserted in the inner spongy titanium powder of placing (7) of retort pipe (3), and retort pipe (3) is connected with outside pumped vacuum systems (8).
2. a kind of titanium sponge hydrogenant vacuum oven device that is used for according to claim 1, it is characterized in that the position that described retort pipe (3) outer wall contacts with furnace wall (1) upper end open is provided with the thermoscreen (9) that prevents that internal heat is scattered and disappeared, described hydrogen tube (6) is inserted on spongy titanium powder (7) wall partly and offers a plurality of equally distributed apertures (10).
3. a kind of titanium sponge hydrogenant vacuum oven device that is used for according to claim 1, it is characterized in that described heating unit (2) is for a plurality of, be distributed in sidewall and bottom in the furnace wall (1), and each heating unit (2) is connected with a thermopair (11) that is used to monitor its temperature variation and control its power.
4. one kind is utilized above-mentioned vacuum oven device to carry out titanium sponge hydrogenant method, it is characterized in that comprising the following steps:
A, spongy titanium powder to be processed is packed in the retort pipe, whether other utility appliance of corresponding inspection is intact, prepares to start start;
B, open outside pumped vacuum systems, in the given time, vacuum tightness reaches 10
-2-10
-3Pa opens heating unit simultaneously, is rapidly heated 270 ℃-320 ℃ the time when thermopair monitors temperature, feeds hydrogen in the retort pipe;
C, hydrogen and spongy titanium powder react, and are heated to 630 ℃-670 ℃ and be incubated 1.5-2.5 hour, and hydrogen pressure remains on 0.15-0.25MPa, begin to be cooled to 280 ℃-320 ℃ subsequently after, end logical hydrogen;
D, when being cooled to 180 ℃-220 ℃, by hoisting ring the retort pipe is hung furnace wall, and the retort pipe is cooled to room temperature, simultaneously, be placed on fully in the refrigerative furnace wall installing the retort pipe for the treatment of the hydrogen treatment spongy titanium powder, carry out the hydrogenation of next batch spongy titanium powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100576192A CN102161473B (en) | 2011-03-10 | 2011-03-10 | Vacuum furnace device for sponge titanium hydrogenation and hydrogenation method of sponge titanium |
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| CN2011100576192A CN102161473B (en) | 2011-03-10 | 2011-03-10 | Vacuum furnace device for sponge titanium hydrogenation and hydrogenation method of sponge titanium |
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| CN102161473A true CN102161473A (en) | 2011-08-24 |
| CN102161473B CN102161473B (en) | 2012-11-21 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102602888A (en) * | 2012-03-19 | 2012-07-25 | 上海华友金镀微电子有限公司 | Production equipment and production method for foamed aluminum foaming agent titanium hydride |
| CN104176762A (en) * | 2014-07-02 | 2014-12-03 | 北京理工大学 | Method for preparing light rare earth deuteride by high-temperature direct process |
| CN105195750A (en) * | 2015-10-16 | 2015-12-30 | 北京工业大学 | Preparation method of micro low-oxygen titanium hydride powder |
| CN106077671A (en) * | 2016-08-29 | 2016-11-09 | 贵州省钛材料研发中心有限公司 | Hydrogenation device for producing titanium powder by hydrogenation dehydrogenation method |
| CN107640744A (en) * | 2017-09-15 | 2018-01-30 | 四川大学 | A kind of unsaturated hydride powder of high-mouldability and preparation method thereof |
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| JP2008001527A (en) * | 2006-06-20 | 2008-01-10 | Toho Titanium Co Ltd | Apparatus for producing titanium hydride or titanium powder and method for producing the same using the apparatus |
| CN101439409A (en) * | 2008-12-29 | 2009-05-27 | 宝鸡迈特钛业有限公司 | Technique for preparing low-oxygen high-purity titanium powder by novel HDH method |
| CN101648699A (en) * | 2009-07-09 | 2010-02-17 | 刘学晖 | Titanium hydride compound foaming powder and quantitative chemical combination process |
| RU2385837C2 (en) * | 2008-02-28 | 2010-04-10 | Учреждение Российской академии наук Институт структурной макрокинетики и проблем материаловедения РАН | Method of producing titanium hydride and device for realising said method |
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2011
- 2011-03-10 CN CN2011100576192A patent/CN102161473B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008001527A (en) * | 2006-06-20 | 2008-01-10 | Toho Titanium Co Ltd | Apparatus for producing titanium hydride or titanium powder and method for producing the same using the apparatus |
| RU2385837C2 (en) * | 2008-02-28 | 2010-04-10 | Учреждение Российской академии наук Институт структурной макрокинетики и проблем материаловедения РАН | Method of producing titanium hydride and device for realising said method |
| CN101439409A (en) * | 2008-12-29 | 2009-05-27 | 宝鸡迈特钛业有限公司 | Technique for preparing low-oxygen high-purity titanium powder by novel HDH method |
| CN101648699A (en) * | 2009-07-09 | 2010-02-17 | 刘学晖 | Titanium hydride compound foaming powder and quantitative chemical combination process |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102602888A (en) * | 2012-03-19 | 2012-07-25 | 上海华友金镀微电子有限公司 | Production equipment and production method for foamed aluminum foaming agent titanium hydride |
| CN104176762A (en) * | 2014-07-02 | 2014-12-03 | 北京理工大学 | Method for preparing light rare earth deuteride by high-temperature direct process |
| CN105195750A (en) * | 2015-10-16 | 2015-12-30 | 北京工业大学 | Preparation method of micro low-oxygen titanium hydride powder |
| CN106077671A (en) * | 2016-08-29 | 2016-11-09 | 贵州省钛材料研发中心有限公司 | Hydrogenation device for producing titanium powder by hydrogenation dehydrogenation method |
| CN107640744A (en) * | 2017-09-15 | 2018-01-30 | 四川大学 | A kind of unsaturated hydride powder of high-mouldability and preparation method thereof |
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| CN102161473B (en) | 2012-11-21 |
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