CN103695674A - Method for preparing Al-Ti-B (aluminum-titanium-boron intermediate) alloy from titanium hydride and potassium fluoborate - Google Patents
Method for preparing Al-Ti-B (aluminum-titanium-boron intermediate) alloy from titanium hydride and potassium fluoborate Download PDFInfo
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- CN103695674A CN103695674A CN201310725538.4A CN201310725538A CN103695674A CN 103695674 A CN103695674 A CN 103695674A CN 201310725538 A CN201310725538 A CN 201310725538A CN 103695674 A CN103695674 A CN 103695674A
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Abstract
The invention discloses a method for preparing an Al-Ti-B (aluminum-titanium-boron intermediate) intermediate alloy refiner from titanium hydride and potassium fluoborate. The preparation method comprises the following steps: weighing 1 to 10 mass percent of dried titanium hydride, 8 to 15 mass percent of potassium fluoborate powder and 75 to 90 mass percent of industrial pure aluminum blocks; placing the aluminum blocks in a crucible, heating the aluminum blocks to 730 to 950 DEG C for melting, sequentially adding the titanium hydride and the potassium fluoborate powder, uniformly stirring the mixture at speed of 100 to 600 rpm, and preserving the heat to obtain aluminum alloy melt; purifying the aluminum alloy melt, pouring and discharging the purified aluminum alloy melt out of a furnace at temperature of 700 to 950 DEG C, and performing water cooling to obtain an Al-Ti-B intermediate alloy. The preparation method has the advantages that a production process is simple, the raw materials are extensive, a small amount of harmful fluoride is emitted, and the microstructure of the prepared Al-Ti-B intermediate alloy contains ideal TiAl3 and TiB2 second-phase particles.
Description
Technical field
The invention belongs to metallurgical smelting field, be specifically related to a kind of method of preparing Al-Ti-B intermediate alloy with titanium hydride and potassium fluoborate.
Background technology
Al-Ti-B master alloy fining agent is the most widely used aluminium and aluminum grain refiner at present, and the aluminium industrial application Al-Ti-B master alloy in the whole world nearly 75% carries out grain refining.The method of producing at present Al-Ti-B master alloy is many, industrial employing be mainly villiaumite method.Villiaumite method is that the basic metal villiaumite of Ti and B is added in molten aluminum melt with certain proportion, through certain technique, form Al-Ti-B master alloy, but the raw material using in villiaumite method is fluorochemicals, especially the addition of potassium fluotitanate reaches 10%, in reaction, emit a large amount of fluorochemicals, healthy all extremely harmful to environment and operator, the preparation of potassium fluotitanate simultaneously also causes certain pollution to environment.Therefore be badly in need of a kind of method of the eco-friendly Al-Ti-B of preparation master alloy.For this reason, develop a kind of method of preparing Al-Ti-B intermediate alloy with titanium hydride and potassium fluoborate.
Summary of the invention
The object of the invention is in order to solve villiaumite legal system for the problem of a large amount of discharges of fluoride obnoxious flavour in the method for Al-Ti-B master alloy fining agent, can obtain again required Al-Ti-B master alloy, thereby a kind of method of preparing Al-Ti-B master alloy with titanium hydride and potassium fluoborate is provided simultaneously.
The object of the present invention is achieved like this, comprises the steps:
A, amount takes the titanium hydride that 1% ~ 10% drying crosses, 8% ~ 15% potassium fluoborate powder, 75% ~ 90% technical pure aluminium block by mass percentage;
B, the aluminium block that A step is taken are put into crucible and are heated to 730 ℃ ~ 950 ℃ and make aluminium block fusing, then add successively titanium hydride and potassium fluoborate powder, and stir with the speed of 100rpm ~ 600rpm, and then insulation, obtains aluminium alloy melt;
C, the aluminium alloy melt that step B is obtained purify, then the aluminium alloy melt after purifying is cast and come out of the stove at the temperature of 700 ℃ ~ 950 ℃, carry out water-cooled, obtain Al-Ti-B intermediate alloy.
The present invention be take titanium hydride, potassium fluoborate and commercial-purity aluminium and is prepared Al-Ti-B master alloy as raw material, has production technique simple, starting material wide material sources, obnoxious flavour fluorochemical discharge capacity is little, in the Al-Ti-B master alloy microtexture of preparation containing desirable TiAl
3and TiB
2second Phase Particle, wherein TiB
2particle is tiny, is particulate state, and mean sizes is less than 5um; TiAl
3for bulk, size is less than the advantages such as 30um.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but never in any form the present invention is limited, and any conversion of doing based on training centre of the present invention, all falls into protection domain of the present invention.
The present invention be take titanium hydride, potassium fluoborate and commercial-purity aluminium and is prepared Al-Ti-B master alloy as raw material, comprises the steps:
A, amount takes the titanium hydride that 1% ~ 10% drying crosses, 8% ~ 15% potassium fluoborate powder, 75% ~ 90% technical pure aluminium block by mass percentage;
B, the aluminium block that A step is taken are put into crucible and are heated to 730 ℃ ~ 950 ℃ and make aluminium block fusing, then add successively titanium hydride and potassium fluoborate powder, and stir with the speed of 100rpm ~ 600rpm, and then insulation, obtains aluminium alloy melt;
C, the aluminium alloy melt that step B is obtained purify, then the aluminium alloy melt after purifying is cast and come out of the stove at the temperature of 700 ℃ ~ 950 ℃, carry out water-cooled, obtain Al-Ti-B intermediate alloy.
The amount by mass percentage of the described A step titanium hydride that preferably 3% ~ 5% drying is crossed, 10% ~ 12% potassium fluoborate.
The titanium hydride powder bake out temperature of described A step is 35 ℃ ~ 45 ℃, and drying time is greater than 1 hour.
Described B step adds titanium hydride and potassium fluoborate powder with graphite bell jar, to add rapidly furnace bottom for first titanium hydride being bundled into several parcels of equivalent with aluminium foil successively, uniform stirring, then add potassium fluoborate.
The holding temperature of described B step is 700 ℃ ~ 950 ℃, and the time is 15min ~ 60min.
The scavenging process of described C step is degasification and pulls out slag, in melt, adds refining agent stirring 2 minutes, standing 8 minutes.
Embodiment 1
Titanium hydride, at 35 ℃, is dried 1 hour, standby; Taking 780 g fine aluminium pieces puts into crucible and is heated to 750 ℃ and makes fine aluminium piece fusing, then add successively titanium hydride 23 g and potassium fluoborate powder 68 g after oven dry, titanium hydride powder is bundled into several parcels of equivalent with aluminium foil and adds rapidly furnace bottom with graphite bell jar, and stir with the speed of 300rpm, add again potassium fluoborate, and stir with the speed of 100rpm ~ 600rpm, then under the condition of 750 ℃, be incubated 30min, obtain aluminium alloy melt; Then aluminium alloy melt is purified, add refining agent and stir 2min with 300rpm, standing 8min, then skims, then aluminium alloy melt is cast and come out of the stove at the temperature of 800 ℃, carries out water-cooled, obtains Al-Ti-B master alloy fining agent.TiAl in its alloy
3and TiB
2second Phase Particle form is good, TiAl
3it is long block that particle is, and mean sizes is less than 30um, distribution disperse.TiB
2particle is particulate state, and size is less than 5um, and distribution uniform.The Al-Ti-B master alloy fining agent thinning effect obtaining is general.
Embodiment 2
Titanium hydride, at 35 ℃, is dried 1 hour, standby; Taking 780 g fine aluminium pieces puts into crucible and is heated to 750 ℃ and makes fine aluminium piece fusing, then add successively titanium hydride 31g and potassium fluoborate powder 77g after oven dry, titanium hydride powder is bundled into several parcels of equivalent with aluminium foil and adds rapidly furnace bottom with graphite bell jar, and stir with the speed of 300rpm, add again potassium fluoborate, and stir with the speed of 100rpm ~ 600rpm, then under the condition of 800 ℃, be incubated 30min, obtain aluminium alloy melt; Right aluminium alloy melt purifies, and adds refining agent and stirs 2min with 300rpm, and standing 8min, then skims, then aluminium alloy melt is cast and come out of the stove at the temperature of 800 ℃, carries out water-cooled, obtains Al-Ti-B master alloy fining agent.TiAl in its alloy
3and TiB
2second Phase Particle form is good, and TiAl
3it is block that particle is, and mean sizes is less than 30um, distribution uniform.TiB
2particle is particulate state, and size is less than 5um, and distribution uniform.The Al-Ti-B master alloy fining agent thinning effect obtaining is better.
Embodiment 3
Titanium hydride, at 35 ℃, is dried 1 hour, standby; Taking 780 g fine aluminium pieces puts into crucible and is heated to 750 ℃ and makes fine aluminium piece fusing, then add successively titanium hydride 39g and potassium fluoborate powder 87g after oven dry, titanium hydride powder is bundled into several parcels of equivalent with aluminium foil and adds rapidly furnace bottom with graphite bell jar, and stir with the speed of 300rpm, add again potassium fluoborate, and stir with the speed of 100rpm ~ 600rpm, then under the condition of 850 ℃, be incubated 30min, obtain aluminium alloy melt; Right aluminium alloy melt purifies, and adds refining agent and stirs 2min with 300rpm, and standing 8min, then skims, then aluminium alloy melt is cast and come out of the stove at the temperature of 800 ℃, carries out water-cooled, obtains Al-Ti-B master alloy fining agent.TiAl in its alloy
3and TiB
2second Phase Particle form is good, and TiAl
3it is block that particle is, and mean sizes is less than 30um, is evenly distributed.TiB
2particle is particulate state, and size is less than 5um, and distribution uniform.The Al-Ti-B master alloy fining agent thinning effect obtaining is better.
Embodiment 4
Titanium hydride, at 35 ℃, is dried 1 hour, standby; Taking 780 g fine aluminium pieces puts into crucible and is heated to 750 ℃ and makes fine aluminium piece fusing, then add successively titanium hydride 47g and potassium fluoborate powder 96g after oven dry, titanium hydride powder is bundled into several parcels of equivalent with aluminium foil and adds rapidly furnace bottom with graphite bell jar, and stir with the speed of 300rpm, add again potassium fluoborate, and stir with the speed of 100rpm ~ 600rpm, then under the condition of 800 ℃, be incubated 50min, obtain aluminium alloy melt; Right aluminium alloy melt purifies, and adds refining agent and stirs 2min with 300rpm, and standing 8min, then skims, then aluminium alloy melt is cast and come out of the stove at the temperature of 800 ℃, carries out water-cooled, obtains Al-Ti-B master alloy fining agent.TiAl in its alloy
3and TiB
2second Phase Particle form is good, and TiAl
3particle is petal-shaped, and mean sizes is less than 30um, distribution uniform.TiB
2particle becomes particulate state, and size is less than 5um, and is evenly distributed.The Al-Ti-B master alloy fining agent thinning effect obtaining is better.
Embodiment 5
Titanium hydride, at 35 ℃, is dried 1 hour, standby; Taking 780 g fine aluminium pieces puts into crucible and is heated to 750 ℃ and makes fine aluminium piece fusing, then add successively titanium hydride 56g and potassium fluoborate powder 106g after oven dry, titanium hydride powder is bundled into several parcels of equivalent with aluminium foil and adds rapidly furnace bottom with graphite bell jar, and stir with the speed of 300rpm, add again potassium fluoborate, and stir with the speed of 100rpm ~ 600rpm, then under the condition of 800 ℃, be incubated 50min, obtain aluminium alloy melt; Right aluminium alloy melt purifies, and adds refining agent and stirs 2min with 300rpm, and standing 8min, then skims, then aluminium alloy melt is cast and come out of the stove at the temperature of 800 ℃, carries out water-cooled, obtains Al-Ti-B master alloy fining agent.TiAl in its alloy
3and TiB
2second Phase Particle form is good, and TiAl
3particle is petal-shaped, and mean sizes is less than 30um, distribution uniform.TiB
2particle becomes particulate state, and size is less than 5um, but is distributed with local clustering phenomena.The Al-Ti-B master alloy fining agent thinning effect obtaining is better.
Embodiment 6
Titanium hydride, at 35 ℃, is dried 1 hour, standby; Taking 780 g fine aluminium pieces puts into crucible and is heated to 750 ℃ and makes fine aluminium piece fusing, then add successively titanium hydride 62g and potassium fluoborate powder 116g after oven dry, titanium hydride powder is bundled into several parcels of equivalent with aluminium foil and adds rapidly furnace bottom with graphite bell jar, and stir with the speed of 300rpm, add again potassium fluoborate, and stir with the speed of 100rpm ~ 600rpm, then under the condition of 800 ℃, be incubated 50min, obtain aluminium alloy melt; Right aluminium alloy melt purifies, and adds refining agent and stirs 2min with 300rpm, and standing 8min, then skims, then aluminium alloy melt is cast and come out of the stove at the temperature of 800 ℃, carries out water-cooled, obtains Al-Ti-B master alloy fining agent.TiAl in its alloy
3and TiB
2second Phase Particle form is poor, and TiAl
3particle is strip, and mean sizes is less than 30um, skewness.TiB
2particle becomes particulate state, and size is less than 5um, exists and assembles.The Al-Ti-B master alloy fining agent thinning effect obtaining is bad.
Claims (6)
1. with titanium hydride and potassium fluoborate, prepare a method for Al-Ti-B intermediate alloy, it is characterized in that comprising the steps:
A, amount takes the titanium hydride that 1% ~ 10% drying crosses, 8% ~ 15% potassium fluoborate powder, 75% ~ 90% technical pure aluminium block by mass percentage;
B, the aluminium block that A step is taken are put into crucible and are heated to 730 ℃ ~ 950 ℃ and make aluminium block fusing, then add successively titanium hydride and potassium fluoborate powder, and stir with the speed of 100rpm ~ 600rpm, and then insulation, obtains aluminium alloy melt;
C, the aluminium alloy melt that step B is obtained purify, then the aluminium alloy melt after purifying is cast and come out of the stove at the temperature of 700 ℃ ~ 950 ℃, carry out water-cooled, obtain Al-Ti-B intermediate alloy.
2. the method for preparing Al-Ti-B intermediate alloy with titanium hydride and potassium fluoborate according to claim 1, the amount by mass percentage that it is characterized in that described A step is the titanium hydride crossed of 3% ~ 5% drying, 10% ~ 12% potassium fluoborate.
3. the method for preparing Al-Ti-B intermediate alloy with titanium hydride and potassium fluoborate according to claim 1, is characterized in that the titanium hydride powder bake out temperature of described A step is 35 ℃ ~ 45 ℃, and drying time is greater than 1 hour.
4. the method for preparing Al-Ti-B intermediate alloy with titanium hydride and potassium fluoborate according to claim 1, it is characterized in that described B step adds titanium hydride and potassium fluoborate powder with graphite bell jar, to add rapidly furnace bottom for first titanium hydride being bundled into several parcels of equivalent with aluminium foil successively, uniform stirring, then add potassium fluoborate.
5. the method for preparing Al-Ti-B intermediate alloy with titanium hydride and potassium fluoborate according to claim 1, the holding temperature that it is characterized in that described B step is 700 ℃ ~ 950 ℃, the time is 15min ~ 60min.
6. the method for preparing Al-Ti-B intermediate alloy with titanium hydride and potassium fluoborate according to claim 1, the scavenging process that it is characterized in that described C step is degasification and pulls out slag, stirs 2 minutes standing 8 minutes to adding refining agent in melt.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104789811A (en) * | 2015-04-03 | 2015-07-22 | 昆明冶金研究院 | Preparation method of aluminum-titanium-boron intermediate alloy |
| CN105886808A (en) * | 2016-06-21 | 2016-08-24 | 昆明冶金研究院 | Metal additive for aluminum alloy smelting and using method thereof |
| CN106244834A (en) * | 2016-07-30 | 2016-12-21 | 昆明冶金研究院 | A kind of method that boron powder and titantium hydride prepare Al-Ti-B intermediate alloy |
| CN106676337A (en) * | 2017-03-02 | 2017-05-17 | 山东建筑大学 | Aluminum-tantalum-boron intermediate alloy and preparation method thereof |
| CN107034374A (en) * | 2017-04-17 | 2017-08-11 | 中国科学院金属研究所 | A kind of method that villiaumite reaction method prepares Al 5Ti 1B intermediate alloys |
| CN107354330A (en) * | 2017-07-13 | 2017-11-17 | 兰州理工大学 | A kind of preparation method of Al Ti C intermediate alloys |
| CN107604184A (en) * | 2017-09-11 | 2018-01-19 | 哈尔滨理工大学 | Al-Ti-B alloy and preparation method thereof |
| CN106435232B (en) * | 2016-10-13 | 2018-04-13 | 昆明冶金研究院 | A kind of preparation method of aluminum-titanium-boron alloy of control TiAl3 particle sizes and distribution of particles |
| CN109750188A (en) * | 2019-03-21 | 2019-05-14 | 孟静 | Aluminum alloy doors and windows production method |
| CN113320621A (en) * | 2021-07-21 | 2021-08-31 | 湖北航特装备制造股份有限公司 | Assembled low-pressure cast aluminum alloy auxiliary frame and preparation process thereof |
| CN115491535A (en) * | 2022-09-27 | 2022-12-20 | 攀枝花学院 | Al-Ti-B intermediate alloy and preparation method thereof |
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| CN104789811A (en) * | 2015-04-03 | 2015-07-22 | 昆明冶金研究院 | Preparation method of aluminum-titanium-boron intermediate alloy |
| CN105886808A (en) * | 2016-06-21 | 2016-08-24 | 昆明冶金研究院 | Metal additive for aluminum alloy smelting and using method thereof |
| CN106244834A (en) * | 2016-07-30 | 2016-12-21 | 昆明冶金研究院 | A kind of method that boron powder and titantium hydride prepare Al-Ti-B intermediate alloy |
| CN106435232B (en) * | 2016-10-13 | 2018-04-13 | 昆明冶金研究院 | A kind of preparation method of aluminum-titanium-boron alloy of control TiAl3 particle sizes and distribution of particles |
| CN106676337A (en) * | 2017-03-02 | 2017-05-17 | 山东建筑大学 | Aluminum-tantalum-boron intermediate alloy and preparation method thereof |
| CN107034374B (en) * | 2017-04-17 | 2018-12-07 | 中国科学院金属研究所 | A kind of method that villiaumite reaction method prepares Al-5Ti-1B intermediate alloy |
| CN107034374A (en) * | 2017-04-17 | 2017-08-11 | 中国科学院金属研究所 | A kind of method that villiaumite reaction method prepares Al 5Ti 1B intermediate alloys |
| CN107354330A (en) * | 2017-07-13 | 2017-11-17 | 兰州理工大学 | A kind of preparation method of Al Ti C intermediate alloys |
| CN107354330B (en) * | 2017-07-13 | 2018-10-26 | 兰州理工大学 | A kind of preparation method of Al-Ti-C intermediate alloys |
| CN107604184A (en) * | 2017-09-11 | 2018-01-19 | 哈尔滨理工大学 | Al-Ti-B alloy and preparation method thereof |
| CN107604184B (en) * | 2017-09-11 | 2019-08-30 | 哈尔滨理工大学 | Al-Ti-B alloy and preparation method thereof |
| CN109750188A (en) * | 2019-03-21 | 2019-05-14 | 孟静 | Aluminum alloy doors and windows production method |
| CN113320621A (en) * | 2021-07-21 | 2021-08-31 | 湖北航特装备制造股份有限公司 | Assembled low-pressure cast aluminum alloy auxiliary frame and preparation process thereof |
| CN115491535A (en) * | 2022-09-27 | 2022-12-20 | 攀枝花学院 | Al-Ti-B intermediate alloy and preparation method thereof |
| CN115491535B (en) * | 2022-09-27 | 2023-11-24 | 攀枝花学院 | Aluminum-titanium-boron intermediate alloy and preparation method thereof |
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Address after: 650031 No. 86 Yuantong North Road, Yunnan, Kunming Patentee after: Kunming Metallurgical Research Institute Co., Ltd Address before: 650031 No. 86 Yuantong North Road, Yunnan, Kunming Patentee before: Kunming Metallurgical Research Institute |