CN104532044A - Low-cost and high-efficiency Al-Ti-C-Ce refining agent and preparation method thereof - Google Patents
Low-cost and high-efficiency Al-Ti-C-Ce refining agent and preparation method thereof Download PDFInfo
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- CN104532044A CN104532044A CN201410786405.2A CN201410786405A CN104532044A CN 104532044 A CN104532044 A CN 104532044A CN 201410786405 A CN201410786405 A CN 201410786405A CN 104532044 A CN104532044 A CN 104532044A
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- 238000002360 preparation method Methods 0.000 title claims description 29
- 238000007670 refining Methods 0.000 title abstract description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 65
- 239000010936 titanium Substances 0.000 claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 22
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000010439 graphite Substances 0.000 claims abstract description 14
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 13
- 238000004880 explosion Methods 0.000 claims abstract description 8
- 239000000155 melt Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000002893 slag Substances 0.000 claims abstract description 5
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 239000006025 fining agent Substances 0.000 claims description 61
- 239000004411 aluminium Substances 0.000 claims description 53
- 239000000843 powder Substances 0.000 claims description 26
- 229910052719 titanium Inorganic materials 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 11
- 229910010038 TiAl Inorganic materials 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 238000004080 punching Methods 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 10
- 238000002844 melting Methods 0.000 abstract description 3
- 230000008018 melting Effects 0.000 abstract description 3
- 238000005266 casting Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 abstract 2
- 229910010039 TiAl3 Inorganic materials 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 14
- 229910052761 rare earth metal Inorganic materials 0.000 description 14
- 238000004445 quantitative analysis Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 229910021383 artificial graphite Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 240000003936 Plumbago auriculata Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000009702 powder compression Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a low-cost and high-efficiency Al-Ti-C-Ce refining agent comprising the following components in percentage by mass: 4.0-16.0% of Ti, 0.5-3.0% of C, 0.5-2.0% of Ce and the balance of Al; and a material phase composition of the refining agent comprises alpha-Al, TiAl3, TiC and Ti2Al20Ce. The Al-Ti-C-Ce refining agent provided by the invention is prepared by adopting an aluminum melt thermal explosion method, and the aluminum melt thermal explosion method mainly comprises the following process steps: (1) preparing raw materials: weighing aluminum powder, titanium powder, graphite powder, aluminum ingots and cerium ingots according to component requirements; (2) uniformly mixing the aluminum powder, the titanium powder and the graphite powder, and pressing to form blocks; (3) heating and melting the aluminum ingots, and then synchronously pressing the cerium ingots and the blocks prepared in the step (2) into aluminum melts by using a graphite clock cover to perform reaction; and (4) filtering the melts, removing molten slag, and casting to obtain Al-Ti-C-Ce refining agent products.
Description
Technical field
The invention belongs to fining agent technical field, relate to a kind of low-cost high-efficiency Al-Ti-C-Ce fining agent and preparation method thereof.
Background technology
Adding grain-refining agent not only can refinement as-cast grain, and refinement dendritic structure, can also reduce loose, reduces hot cracking tendency, reduces casting flaw, improves follow-up processing characteristics.In recent years along with the research to aluminium alloy fining agent, develop Al-Ti-C grain-refining agent.TiC particle in Al-Ti-C grain-refining agent is little because of size, not easily assembles, is evenly distributed, and have the advantages such as good coherency with Al, and be subject to extensive concern.But because the wettability of C in Al is poor, prepare very difficult, prepare Al-Ti-C grain-refining agent by violent stirring or pyroreaction, preparation cost is higher, limits the widespread use of Al-Ti-C grain-refining agent.
At present, various countries researchist develops the preparation of multiple method for AI-Ti-C fining agent.But use for reference and prepare the method adding rare earth in Al-Ti-B refiner process, the research report of preparation Al-Ti-C-Ce fining agent is few.The grain refining efficiency of the Al-Ti-C-RE fining agent that the Zhao Hongliang of Zhengzhou University etc. prepare is better than AI-Ti-C fining agent, and it is long-lasting to have good refinement.But the preparation method developed still exists some shortcomings, as when adopting potassium fluotitanate to introduce Ti element, produce a large amount of fluoride gas contaminate environment in preparation process, etching apparatus, and easily form the metallurgical quality that villiaumite inclusion affects fining agent; In addition, preparation temperature higher (about 1250 DEG C), needs melting in induction furnace, and scaling loss is serious, and energy consumption is larger.Zhao Hongliang etc. provide Ti element at employing titanium sponge for raw material, and when adopting resistance furnace to prepare Al-Ti-C-RE fining agent, preparation temperature is higher (about 950 DEG C) still, and energy consumption is still comparatively large, and preparation cost is higher.
Summary of the invention
The object of the invention is to for prior art Problems existing, provide a kind of low cost and efficient Al-Ti-C-Ce fining agent.
Another object of the present invention is to the preparation method that a kind of above-mentioned Al-Ti-C-Ce fining agent is provided.
For this reason, the present invention adopts following technical scheme:
A kind of low-cost high-efficiency Al-Ti-C-Ce fining agent, comprise following mass percent component, Ti:4.0-16.0%, C:0.5-3.0%, Ce:0.5-2.0%, surplus is Al; The thing phase composite of described fining agent comprises α-Al, TiAl
3, TiC and Ti
2al
20ce.
A preparation method for above-mentioned Al-Ti-C-Ce fining agent, adopts Thermal explosion method in aluminum liquid preparation, specifically comprises following processing step:
(1) raw material prepares, and weighs aluminium powder, titanium valve, Graphite Powder 99, aluminium ingot, cerium ingot, require that the mol ratio of aluminium powder and titanium valve and Graphite Powder 99 is 1:0.2-0.8:0.1-0.6, aluminium ingot purity requirement 99.9% by component requirements; Cerium ingot purity requirement 99.9%;
(2) load weighted aluminium powder, titanium valve, Graphite Powder 99 are mixed, be placed in mould, be pressed into block;
(3) aluminium ingot is heated to 780 ~ 850 DEG C, after aluminium ingot melts completely, graphite bell jar is pressed into cerium ingot and the obtained block of step (2) in molten aluminium simultaneously; Until cerium ingot and block by molten aluminium preheating vigorous reaction after completing reaction, leave standstill 5-8 minute, to leave standstill in process the interior graphite rod of per minute to melt strong stirring once;
(4) filtered by the strumbox of the alloy melt of step (3) with preheating, removing slag, by melt cast in punching block, obtains Al-Ti-C-Ce fining agent product.
Further, in step (1), the granularity requirements of described feed metal powder is, aluminium powder 200 order, titanium valve 350 order, Graphite Powder 99 400 order.
Further, in step (1), during raw material weighing, require that the mol ratio of titanium valve and Graphite Powder 99 is 2:1.
Further, in step (4), the preheating temperature of described strumbox is 450-550 DEG C.
Preparation method of the present invention adopts Thermal explosion method in aluminum liquid, belongs to the one of Self-propagating Sintering Synthetic method, and namely utilizing the energy of high thermopositive reaction to make, the chemical reaction of two or more material pressed compact is automatic continuous spreads down, generates the method for compound.In the inventive method, aluminium powder, titanium valve, Graphite Powder 99 mixed and directly joins in molten aluminium after being pressed into block, causing the thermopositive reaction between aluminium, titanium, graphite three kinds of elements by the heat of molten aluminium; Thermopositive reaction makes molten aluminium temperature raise, and can ensure the fusing of cerium ingot and participate in reaction.The whole reaction process time is shorter, takes full advantage of the thermopositive reaction of raw material, reduces preparation temperature.
Rare earth element is surfactant, adds the surface energy that can reduce aluminium in molten aluminium to, crystal grain thinning and dendritic structure: and rare earth element is easily adsorbed on crystal boundary and phase boundary place, hinders growing up of crystal grain; Rare earth element segregation coefficient is comparatively large, easily forms larger constitutional supercooling.Based on numerous refinement advantage and the metamorphism thereof of rare earth, in the process of preparation Al-Ti-C grain-refining agent, add rare earth element, can improve the wettability of C in aluminium, thus improve reaction efficiency, preparation is fining agent more efficiently.The present invention's cost-efficiently Al-Ti-C-Ce fining agent that namely utilized Thermal explosion method in aluminum liquid successfully to prepare.
For further analysis below by X-ray diffraction analysis, scanning electron microscope analysis and the thing phase quantitative analysis stuctures and properties to Al-Ti-C-Ce fining agent prepared by the present invention.
1, X-ray diffraction analysis
Fig. 1 is that Al-Ti-C-Ce fining agent (b) adopting the inventive method to prepare composes with the XRD figure of comparative example A l-Ti-C fining agent (a).Can find out, Al-Ti-C-Ce fining agent (b) is primarily of α-Al, TiAl
3, TiC, Ti
2al
20ce phase composite.In the fining agent synthesized after adding rare earth element, the peak value of TiC obviously raises, and shows that rare earth element facilitates the formation of TiC particle, number of particles showed increased.
2, scanning electron microscope analysis
Fig. 2-1 is the SEM figure of Al-Ti-C-Ce fining agent prepared by the present invention, and blocky particles a large amount of as seen in figure, the small-particle of sheet distribution, a kind of contrast is brighter, is Ti
2al
20ce, TiAl
3; A kind of contrast is comparatively dark, is TiC.In Fig. 2-1, the particle of size bulk below 10 μm is TiAl
3particle; Size is below 0.5 μm, and the particle that grain boundaries distributes in the form of sheets is TiC particle, and the particle of size bulk more than 10 μm is Ti
2al
20ce particle.Fig. 2-2 is the SEM figure not adding Al-Ti-C fining agent prepared by rare earth.Contrast visible, the TiC number of particles showed increased distributed in the form of sheets after adding rare earth element, shows that rare earth element facilitates the formation of TiC particle, is conducive to the thinning effect of REINFORCED Al-Ti-C fining agent.
3, thing phase quantitative analysis
The thing phase quantitative analysis of the Al-Ti-C-Ce fining agent that Fig. 5-7 is prepared for the present invention, can find out due to after with the addition of rare earth element ce in fining agent, define more Ti
2al
20ce phase, and its contrast and TiAl
3substantially identical.
4, fining agent effect analysis
Fig. 8 and 9 is that Al-Ti-C-Ce and the Al-Ti-C fining agent of interpolation 0.5% carries out the macrostructure after refinement to commercial-purity aluminium.Can find out, after the fining agent adding identical amount, the thinning effect of Al-Ti-C-Ce fining agent is obviously better than Al-Ti-C fining agent, and grain-size is less than 100 μm.
To sum up, the thinning effect of Al-Ti-C-Ce fining agent of the present invention is obviously better than Al-Ti-C fining agent; Compared with preparation method of the present invention contains rare earth element fining agent preparation method with tradition, reduce preparation feedback temperature, greatly shorten reaction preparation time, not only reduce preparation cost, and solve the difficult problem of TiC particle preparation, the interpolation of Rare-Earth Ce, improve the wettability of C in Al, facilitate the generation of TiC, improve reaction efficiency, make Al-Ti-C-Ce fining agent of the present invention have low cost and efficient feature.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the Al-Ti-C-Ce for preparing of the present invention and comparative example A l-Ti-C fining agent;
Fig. 2-1 is SEM collection of illustrative plates when Al-Ti-C-Ce fining agent prepared by the present invention amplifies 500 times;
Fig. 2-2 is the SEM collection of illustrative plates of comparative example A l-Ti-C fining agent when amplifying 500 times;
Fig. 3 is Al-Ti-C-Ce fining agent prepared by the present invention SEM collection of illustrative plates when amplifying 1000 times;
Fig. 4 is the SEM collection of illustrative plates of Al-Ti-C-Ce fining agent prepared by the present invention TiC when amplifying 3000 times;
Fig. 5 is Ti in Al-Ti-C-Ce fining agent of the present invention
2al
20the thing phase quantitative analysis of Ce;
Fig. 6 is TiAl in Al-Ti-C-Ce fining agent of the present invention
3thing phase quantitative analysis;
Fig. 7 is the thing phase quantitative analysis of TiC in Al-Ti-C-Ce fining agent of the present invention;
Fig. 8 is that the Al-Ti-C-Ce fining agent of interpolation 0.5% is to the macrostructure after commercial-purity aluminium refinement;
Fig. 9 is that the Al-Ti-C fining agent of interpolation 0.5% is to the macrostructure after commercial-purity aluminium refinement;
In Fig. 3-4, A is Ti
2al
20ce phase, B is TiAl
3phase, C is TiC phase.
Embodiment
embodiment 1
It is as follows that Thermal explosion method in aluminum liquid prepares Al-Ti-C-Ce fining agent process:
(1) raw material prepares, and fining agent is prepared by aluminium powder, titanium valve, Graphite Powder 99, aluminium ingot, cerium ingot.Weigh aluminium powder, titanium valve, Graphite Powder 99, aluminium ingot, cerium ingot by component requirements, require that the mol ratio of aluminium powder and titanium valve and Graphite Powder 99 is 1:0.8:0.4; Aluminium ingot purity 99.9%, cerium ingot purity 99.9%; Powder size: Al powder 200 order, Ti powder 350 order, C powder 400 order.
(2) aluminium powder, titanium valve, powdered graphite are mixed, the powder mixed is placed in mould, apply the pressure of 60MPa, be pressed into the cylindricality block of φ 25 × 50.
(3) plumbago crucible is selected to carry out melting, graphite rod stirs, and prevents the pollution of Si, utilizes well formula resistance furnace that clean aluminium ingot is heated to 800 DEG C, after aluminium ingot melts completely, graphite bell jar is pressed into cerium ingot and step (2) block simultaneously, and cerium ingot and block, by molten aluminium preheating, vigorous reaction occurs, and the reaction times is about 1-3 minute, after question response completes, leave standstill 5 minutes, leave standstill the interior artificial graphite rod of per minute in process to melt strong stirring once, stir 5 times;
(4) filtered by the alloy melt of the acquisition strumbox being preheated to 500 DEG C, removing slag, by melt cast in punching block, obtains Al-Ti-C-Ce fining agent.
In said process, by the instrument such as mould and strumbox brushing one coating, prevent Fe impurity element from polluting fining agent.
embodiment 2
Embodiment 2 is with the difference of embodiment 1:
In step (1), the mol ratio of aluminium powder and titanium valve and Graphite Powder 99 is 1:0.2:0.6;
In step (3), utilize well formula resistance furnace that clean aluminium ingot is heated to 780 DEG C, after aluminium ingot melts completely, graphite bell jar is pressed into cerium ingot and step (2) block simultaneously; After having reacted, leave standstill 8 minutes, every 1 minute artificial graphite rod to melt strong stirring once, stirs 8 times;
In step (4), the preheating temperature of strumbox is 450 DEG C.
embodiment 3
Embodiment 3 is with the difference of embodiment 1:
In step (1), the mol ratio of aluminium powder and titanium valve and Graphite Powder 99 is 1:0.4:0.1;
In step (3), utilize well formula resistance furnace that clean aluminium ingot is heated to 850 DEG C, after aluminium ingot melts completely, graphite bell jar is pressed into cerium ingot and step (2) block simultaneously; After having reacted, leave standstill 6 minutes, every 1 minute artificial graphite rod to melt strong stirring once, stirs 6 times;
In step (4), the preheating temperature of strumbox is 550 DEG C.
comparative example
A kind of Al-Ti-C fining agent, its mass percent component is: Ti:5%, C:0.63%, and surplus is Al.The process that employing Thermal explosion method in aluminum liquid prepares described Al-Ti-C fining agent is as follows:
Aluminium ingot, aluminium powder, titanium valve, Graphite Powder 99 are pressed component requirements proportioning, requires that the mol ratio of aluminium powder and titanium valve and Graphite Powder 99 is 1:0.4:0.2 simultaneously; Above-mentioned powder compression is become the cylindricality powder agglomates of 25 × 50.
Utilize well formula resistance furnace that clean aluminium ingot is heated to 780 DEG C, treat that aluminium ingot melts completely, the cylindricality powder agglomates press-in molten aluminium will suppressed in advance with graphite bell jar, graphite rod uniform stirring, makes it that combustion reactions occur, after complete reaction; Leave standstill 5min; Slag and the oxide skin on surface is removed with spoon of skimming; Be poured in punching block, obtain Al-Ti-C fining agent.
Claims (5)
1. a low-cost high-efficiency Al-Ti-C-Ce fining agent, is characterized in that, comprises following mass percent component, Ti:4.0-16.0%, C:0.5-3.0%, Ce:0.5-2.0%, and surplus is Al; The thing phase composite of described fining agent comprises α-Al, TiAl
3, TiC and Ti
2al
20ce.
2. a preparation method for Al-Ti-C-Ce fining agent described in claim 1, is characterized in that, adopts Thermal explosion method in aluminum liquid preparation, specifically comprises following processing step:
(1) raw material prepares, and weighs aluminium powder, titanium valve, Graphite Powder 99, aluminium ingot, cerium ingot, require that the mol ratio of aluminium powder and titanium valve and Graphite Powder 99 is 1:0.2-0.8:0.1-0.6, aluminium ingot purity requirement 99.9% by component requirements; Cerium ingot purity requirement 99.9%;
(2) load weighted aluminium powder, titanium valve, Graphite Powder 99 are mixed, be placed in mould, be pressed into block;
(3) aluminium ingot is heated to 780 ~ 850 DEG C, after aluminium ingot melts completely, graphite bell jar is pressed into cerium ingot and the obtained block of step (2) in molten aluminium simultaneously; Until cerium ingot and block by molten aluminium preheating vigorous reaction after completing, leave standstill 5-8 minute, to leave standstill in process the interior graphite rod of per minute to melt strong stirring once;
(4) alloy melt step (3) the obtained strumbox of preheating filters, and removing slag, by melt cast in punching block, obtains Al-Ti-C-Ce fining agent product.
3. the preparation method of a kind of Al-Ti-C-Ce fining agent according to claim 2, is characterized in that, in step (1), the granularity requirements of described feed metal powder is, aluminium powder 200 order, titanium valve 350 order, Graphite Powder 99 400 order.
4. the preparation method of a kind of Al-Ti-C-Ce fining agent according to claim 2, is characterized in that, in step (1), during raw material weighing, requires that the mol ratio of titanium valve and Graphite Powder 99 is 2:1.
5. the preparation method of a kind of Al-Ti-C-Ce fining agent according to claim 2, is characterized in that, in step (4), the preheating temperature of described strumbox is 450-550 DEG C.
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Cited By (9)
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CN106756146A (en) * | 2016-11-24 | 2017-05-31 | 兰州理工大学 | A kind of preparation method of Al Ti C Ce fining agents |
CN107326228A (en) * | 2017-06-23 | 2017-11-07 | 兰州理工大学 | A kind of composite inoculating transcocrystallized Al-Si alloy and preparation method thereof |
CN108018443A (en) * | 2017-06-12 | 2018-05-11 | 吉林大学 | Nanometer TiB for aluminum alloy organization's refinement2Grain refiner and thinning method |
CN108277373A (en) * | 2018-02-07 | 2018-07-13 | 兰州理工大学 | A kind of Al-Ti-C-La alloys and preparation method thereof |
CN108330308A (en) * | 2018-02-07 | 2018-07-27 | 兰州理工大学 | A kind of Al-Ti-C-La composite crystal grain fining agents, alloy and preparation method thereof |
CN112746195A (en) * | 2020-12-30 | 2021-05-04 | 吉林大学 | Recession-resistant refiner, preparation method and application thereof, aluminum alloy and refining method thereof |
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CN114150173A (en) * | 2021-12-07 | 2022-03-08 | 福建省漳平市九鼎氟化工有限公司 | Al-Ti-C-Sc intermediate alloy refiner and preparation method thereof |
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CN107326228A (en) * | 2017-06-23 | 2017-11-07 | 兰州理工大学 | A kind of composite inoculating transcocrystallized Al-Si alloy and preparation method thereof |
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