CN107737941A - TiB for increasing material manufacturing2Strengthen the preparation method of Al alloy powder - Google Patents
TiB for increasing material manufacturing2Strengthen the preparation method of Al alloy powder Download PDFInfo
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- CN107737941A CN107737941A CN201711060637.XA CN201711060637A CN107737941A CN 107737941 A CN107737941 A CN 107737941A CN 201711060637 A CN201711060637 A CN 201711060637A CN 107737941 A CN107737941 A CN 107737941A
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- borofluoride
- fluotitanate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1042—Alloys containing non-metals starting from a melt by atomising
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1089—Alloys containing non-metals by partial reduction or decomposition of a solid metal compound
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The present invention relates to the TiB for increasing material manufacturing2Strengthen the preparation method of Al alloy powder, first weigh fluotitanate and borofluoride respectively, wherein, the mol ratio of B atoms is 1 in Ti atoms and borofluoride in the fluotitanate weighed:2 2.4, mix, grind, dry, it is standby；During vacuum melting aluminium alloy, after each alloy raw material is completely melt, 800 900 DEG C are warming up to, after standing 15 45min, the fluotitanate and borofluoride mixed-powder of preparation are put into aluminium alloy melt, stirs 1 3min, is incubated 30 90min；Powder by atomization is carried out to the melt finally obtained, screening, obtains the TiB for increasing material manufacturing2Strengthen Al alloy powder.TiB in powder of the present invention2Enhancing is mutually reaction generation, and particle size is smaller, reaches nanoscale, and final products increasing material manufacturing powder is more than 15 microns of powder, and enhancing mutually can be uniformly distributed in increasing material manufacturing powder；The fluoaluminate of reaction generation often uses refining agent for aluminium alloy, can purify melt, adsorbs other impurities element, improves Melt parity.
Description
Technical field
The present invention relates to a kind of TiB for increasing material manufacturing2Strengthen the preparation method of Al alloy powder, more particularly, to
The growth in situ TiB of increasing material manufacturing2Strengthen the preparation method of Al alloy powder, belong to increasing material manufacturing field of powder preparation.
Background technology
Increases material manufacturing technology is one kind of rapid shaping technique, and it is a kind of based on threedimensional model, with metal powder
End or plastics etc. can jointing material, by successively scanning, the mode of stacking constructs the technology of stereoscopic three-dimensional part layer by layer.
The technology combines all kinds of subjects such as CAD/CAM, optics, numerical control and material science, and application field is very extensive, in jewelry, doctor
Treatment, footwear, industrial design, building, Aero-Space, automobile, education etc. have application prospect.
Currently for aluminum alloy materials increasing material manufacturing, the dusty material used is relatively more fixed, generally AlSi10Mg,
The alusil alloys such as AlSi7Mg, AlSi12 are in the majority, due to having preferable welding performance, increasing material manufacturing technics comparing maturation.But due to
AlSi series alloy mechanical properties are not high, cause the part mechanical property of increasing material manufacturing also insufficient, it is impossible to meet at present to close aluminium
The requirement of golden increasing material manufacturing part high intensity, it is therefore desirable to be improved to Al alloy powder powder material, improve mechanical property.
In increasing material manufacturing with Al alloy powder development, addition reinforcing particle can improve the mechanics of traditional aluminium alloy
Performance.Therefore, it is necessary to which a kind of suitable process meanses carry the increasing material manufacturing Al alloy powder powder material for strengthening phase to prepare.
Al alloy powder is modified, adding some has the additive of special role, for improving Al alloy powder
Print performance is one of R＆D direction of emphasis.Patent [CN106694870A] is exactly the research and development side that manufacturer is modified to powder
Case, after adding fluoaluminic acid caesium and potassium fluoroaluminate, although having certain improvement to powder print performance and printing part mechanical property,
Due to adding the elements such as caesium and potassium in the powder, and content is not low, and caused fluoride can not exclude completely, therefore can band
Enter impurity, and fluoride is harmful to environment, should not largely be used.
Al alloy powder is post-processed so that there is the generation of aluminum oxide coating on powder surface, for improving aluminium alloy
The print performance of powder is one of R＆D direction of emphasis.Patent [CN106623897A] is exactly that manufacturer is modified to powder
Development Scheme, alumina-coated layer is added on powder surface so that powder turns into aluminum oxide/aluminium composite material, can be one
Determine to improve powder property in scope.But after introducing aluminum oxide, oxygen content in power substantially increases, and 3D printing process is quick to oxygen content
Sense, increase oxygen content can cause other problemses.Secondly, oxidation aluminum surface layer fusing point is higher, and printout there may be after printing shaping
Lamination, it is unfavorable for printout long-term use.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of TiB for increasing material manufacturing2Strengthen the system of Al alloy powder
Preparation Method, aluminium base/TiB is prepared by growth in situ mode2Composite powder, lift the performance of Al alloy powder.
In order to solve the above-mentioned technical problem, technical scheme is as follows：TiB for increasing material manufacturing2Strengthen aluminium to close
The preparation method at bronze end, comprises the following steps：
1）Take fluotitanate and borofluoride；
2）Smelting aluminium alloy, step 1 is put into aluminium alloy melt）The fluotitanate and borofluoride of middle preparation, stirring；
3）To step 2）In melt carry out powder by atomization.
Further, to step 1）In fluotitanate and borofluoride mixing, grind, dry.
Further, step 2）In after each alloy raw material is completely melt, be warming up to 800-900 DEG C, stand 15-45min
Afterwards, step 1 is added）In fluotitanate and borofluoride；The preferred 1-3min of mixing time, 30-90min is incubated after stirring.
Further, screening step is also included after powder by atomization.
Further, the TiB for increasing material manufacturing2Strengthen the preparation method of Al alloy powder, comprise the following steps：
1) fluotitanate and borofluoride are weighed respectively, wherein, B atoms in Ti atoms and borofluoride in the fluotitanate weighed
Mol ratio be 1:2-2.4, mix, grind, dry, it is standby；
2) during vacuum melting aluminium alloy, after each alloy raw material is completely melt, 800-900 DEG C is warming up to, after standing 15-45min,
Step 1 is put into aluminium alloy melt）The fluotitanate and borofluoride mixed-powder of middle preparation, 1-3min is stirred, be incubated 30-
90min；
3) to step 2）In the melt that finally obtains carry out powder by atomization, screening, obtain the TiB for increasing material manufacturing2Strengthen aluminium
Alloy powder.
Step 1）In, the fluotitanate includes Li2TiF6、Na2TiF6、K2TiF6、MgTiF6In one or more.It is excellent
Elect fluotitanic acid haloid, more preferably K as2TiF6。
Step 1）In, the borofluoride includes LiBF4、NaBF4、KBF4In one or more.Preferably fluotitanic acid halogen
Plain salt, more preferably KBF4。
Step 1）In, the mol ratio of B atoms is 1 in Ti atoms and borofluoride in the fluotitanate weighed:2.2.
Step 1）In, fluotitanate and borofluoride mixed-powder are placed in vacuum drying chamber, under the conditions of 180-220 DEG C
Dry 1.5-3h.
Step 2）In, during vacuum melting aluminium alloy, aluminium ingot is put into first, it is then that other alloy raw materials are suitable by fusing point height
Sequence is sequentially placed into secondary batching mouth, by step 1）The fluotitanate and borofluoride mixed-powder of middle preparation are put into the 3rd and fed intake dress
In putting, after each alloy raw material is completely melt, 850 DEG C are warming up to, after standing 30min, by the 3rd charging device to aluminium alloy
Input fluotitanate and borofluoride mixed-powder in melt.
Step 2）In, stir speed (S.S.) is 250 turns/min, mixing time 2min, soaking time 60min.
Step 3）In, by step 2）In finally obtain melt substep pour into tundish, the temperature for keeping tundish is
800-900 DEG C, powder by atomization is carried out, is ordinary skill in the art means to melt atomization powder, it is preferred that atomization gas pressure
Power is 3.8MPa, and draft-tube diameter 3.5mm, working chamber's malleation is in more than 15KPa.
Step 3）In, the dusty material obtained to powder by atomization during screening is classified, and it is 15-53 microns to filter out particle diameter
Powder, obtain the TiB for increasing material manufacturing2Strengthen Al alloy powder finished product.
A kind of TiB for increasing material manufacturing2Strengthen Al alloy powder, be made using preparation method as described above.
During vacuum gas-atomized powder, by adding fluotitanate and borofluoride, preferably by temperature and
The control of the techniques such as soaking time, generates TiB in aluminium alloy melting2Nano-scale particle.Again by gas-atomized powder technology,
Prepared by fused solution turn into dusty material so that the intercrystalline of powder particle has TiB2Particulates reinforcements.From potassium fluotitanate and
Potassium fluoborate is in situ to prepare TiB2When, key reaction equation is as follows：
Preferably, in metal smelting process, TiB is carried out2Growth in situ technique, TiB2Reaction temperature is set in 850 DEG C, reaction
Soaking time is set as 60min.Further, during the course of the reaction, fused solution is stirred, stir speed (S.S.) be 250 turns/
min.Under the conditions of 850 DEG C of temperature, optimum TiB2Generation, reaction 60min can farthest ensure Ti elements and B element
Form TiB2And backward reaction does not occur, stir speed (S.S.), which is set to 250 turns/min, can disperse TiB well2Particle, too fast rotating speed
Established TiB can be lost2Particle, scattered effect is not had then slowly excessively.
Further, to completing growth in situ TiB2During the melt of particle carries out powder by atomization, for melt
The characteristics of sticky, the present invention carry out atomization process using 3.5mm mozzle, and working chamber's malleation ensures liquation in more than 15Kpa
Can smoothly it flow down, and atomizing medium pressure is not less than 3.8Mpa by different spray nozzles structures shape, general admission pressure.
Compared with prior art, beneficial effects of the present invention are as follows：
1）Due to TiB in powder2Enhancing is mutually reaction generation, therefore particle size is smaller, reaches nanoscale, and final products increase material
Manufacture powder is more than 15 microns of powder, therefore enhancing mutually can be uniformly distributed in increasing material manufacturing powder；
2）React the fluoaluminate of generation（Such as potassium fluoroaluminate）Refining agent is often used for aluminium alloy, melt can be purified, adsorb it
His impurity element, improve Melt parity；
3）Reaction generates without other impurities, in the absence of poisonous and harmful product, process environmental protection；
4）Reaction of formation is sensitive to technological parameter, and by controlling smelting technology to be controlled to reaction, production stability is higher；
5）After ceramic particle in fused solution being present liquid can be caused sticky, this programme can ensure that atomization process is smooth.
6）Fabricated in situ and powder by atomization step are combined by the present invention, and preparation flow has been greatly shortened, has reduced system
Standby cost, improves powder property.
Brief description of the drawings
Fig. 1 is free from TiB2Strengthen the SEM figures of 2024 Al alloy powders of phase.
Fig. 2 is the growth in situ TiB of embodiment 12Strengthen 2024 Al alloy powder SEM shape appearance figures of phase.
Fig. 3 is that the EDS of boxed area in Fig. 2 analyzes collection of illustrative plates.
Embodiment
Describe the present invention in detail below with reference to accompanying drawing and in conjunction with the embodiments.It should be noted that in the feelings not conflicted
Under condition, the feature in embodiment and embodiment in the present invention can be mutually combined.
Embodiment 1
Below to prepare in-situ preparation TiB2Strengthen and the present invention is further described exemplified by 2024 Al alloy powders.
Its preparation process comprises the following steps：
1）Dispensing：Increasing material manufacturing powder require composition it is accurate, impurity content is extremely low, therefore, alloy raw material using 99.999% it is pure
Ingot.Configured by 2024 aluminium alloy national standards, surface oxide layer polishing is carried out before feeding intake, polishing, is put into vacuum
120 DEG C of drying box dry 3h, it is standby；
2）Prepare potassium villiaumite：K2TiF6And KBF4By Ti atoms and B atomic molars ratio 1:2.2 dispensings, fine powder shape is ground into,
It is put into the dry 2h of 200 DEG C of vacuum drying chamber；
3）Vacuum melting：Al ingots are put into first, and other alloy raw materials are sorted by fusing point height, secondary batching mouth are put into, by potassium
Villiaumite is put into special 3rd charging device；Conventional smelting technology is used to 2024 alloys, treats alloy molten liquid completely by metal
Melting sources；
4）In-situ preparation TiB2Particle：Melt temperature is promoted to 850 DEG C, stands 30min；Put into by the 3rd charging device
In molten mass, while in the agitating device insertion molten mass that smelting furnace is covered, 2min is stirred with 250 turns/min speed, it
Insulation 60min ensures that reaction is completed afterwards；
5）Powder by atomization：After completing above-mentioned steps, molten mass substep is poured into tundish, it is 850 DEG C to keep tundish temperature, if
It is 3.8MPa to put atomization pressure, and draft-tube diameter 3.5mm, working chamber's malleation is 16KPa, carries out atomization process；
6）Powder classification：Dusty material is classified by increasing material manufacturing powder requirement, bound is respectively that 15 microns and 53 are micro-
Rice, after the completion of screening, obtain TiB2Strengthen 2024 Al alloy powder finished products.
Fig. 1 is without TiB2Strengthen the SEM figures of 2024 Al alloy powders of phase, it is seen then that its powdered ingredients is 2024 conjunctions
Gold, there is no other mutually to generate on powder particle.
Fig. 2 and Fig. 3 is respectively the growth in situ TiB of the present embodiment2Strengthen phase 2024 Al alloy powder SEM shape appearance figures and
The EDS analysis collection of illustrative plates of boxed area in SEM figures, it is seen then that there is obvious white second phase generation on powder surface, is scanned by EDS
It can find that the elements such as Ti, B are contained in the region, white second phase is in-situ preparation TiB2Particle, size are nanoscale.
The content that above-described embodiment illustrates should be understood to that these embodiments are only used for being illustrated more clearly that the present invention, without
For limiting the scope of the present invention, after the present invention has been read, the various equivalent form of values of the those skilled in the art to the present invention
Modification each fall within the application appended claims limited range.
Claims (10)
- A kind of 1. TiB2Strengthen the preparation method of Al alloy powder, it is characterised in that comprise the following steps：1）Take fluotitanate and borofluoride；2）Smelting aluminium alloy, step 1 is put into aluminium alloy melt）The fluotitanate and borofluoride of middle preparation, stirring；3）To step 2）In melt carry out powder by atomization.
- 2. preparation method according to claim 1, it is characterised in that to step 1）In fluotitanate and borofluoride mix Close, grind, dry；And/or it is 1 to control the mol ratios of B atoms in Ti atoms and borofluoride in fluotitanate:2-2.4.
- 3. preparation method according to claim 1, it is characterised in that step 2）In after each alloy raw material is completely melt, 800-900 DEG C is warming up to, after standing 15-45min, adds step 1）In fluotitanate and borofluoride；Mixing time is preferred 1-3min, 30-90min is incubated after stirring.
- 4. preparation method according to claim 1, it is characterised in that step 1）In, the fluotitanate includes Li2TiF6、 Na2TiF6、K2TiF6、MgTiF6In one or more；The borofluoride includes LiBF4、NaBF4、KBF4In one kind or more Kind.
- 5. preparation method according to claim 1, it is characterised in that step 1）In, Ti atoms in the fluotitanate weighed Mol ratio with B atoms in borofluoride is 1:2.2；Fluotitanate and borofluoride mixed-powder are placed in vacuum drying chamber, 1.5-3h is dried under the conditions of 180-220 DEG C.
- 6. preparation method according to claim 1, it is characterised in that step 2）In, during vacuum melting aluminium alloy, throw first Enter aluminium ingot, other alloy raw materials are then sequentially placed into secondary batching mouth by fusing point sequence, by step 1）The fluorine of middle preparation Titanate and borofluoride mixed-powder are put into the 3rd charging device, after each alloy raw material is completely melt, are warming up to 850 DEG C, after standing 30min, fluotitanate and borofluoride mixed-powder are put into aluminium alloy melt by the 3rd charging device.
- 7. preparation method according to claim 1, it is characterised in that step 2）In, stir speed (S.S.) is 250 turns/min, is stirred It is 2min, soaking time 60min to mix the time.
- 8. preparation method according to claim 1, it is characterised in that step 3）In, by step 2）In finally obtain it is molten Body substep pours into tundish, and the temperature for keeping tundish is 800-900 DEG C, carries out powder by atomization, wherein, atomization pressure is 3.8MPa, draft-tube diameter 3.5mm, working chamber's malleation is in more than 15KPa.
- 9. preparation method according to claim 1, it is characterised in that step 3）In, powder by atomization is obtained during screening Dusty material is classified, and is filtered out the powder that particle diameter is 15-53 microns, is obtained the TiB for increasing material manufacturing2Strengthen aluminium alloy Powder product.
- A kind of 10. TiB for increasing material manufacturing2Strengthen Al alloy powder, it is characterised in that using such as any one of claim 1-9 Described preparation method is made.
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| CN201711060637.XA CN107737941A (en) | 2017-11-02 | 2017-11-02 | TiB for increasing material manufacturing2Strengthen the preparation method of Al alloy powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109576496A (en) * | 2018-12-29 | 2019-04-05 | 中北大学 | Waste aluminum recovery prepares method, product and the equipment that powder is used in selective laser fusing |
| CN109692964A (en) * | 2019-01-31 | 2019-04-30 | 中南大学 | A kind of reinforced aluminum matrix composites and preparation method thereof |
| CN110512111A (en) * | 2018-04-11 | 2019-11-29 | 上海交通大学 | The preparation method of in-situ Al-base composition |
| CN111822722A (en) * | 2020-06-30 | 2020-10-27 | 长沙新材料产业研究院有限公司 | TiAl/TiB for additive manufacturing2Method for preparing powder material |
| CN116237542A (en) * | 2023-03-15 | 2023-06-09 | 山东大学 | In-situ generation and non-original addition method, material and application of reinforcing phase of GH3230 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110512111A (en) * | 2018-04-11 | 2019-11-29 | 上海交通大学 | The preparation method of in-situ Al-base composition |
| CN109576496A (en) * | 2018-12-29 | 2019-04-05 | 中北大学 | Waste aluminum recovery prepares method, product and the equipment that powder is used in selective laser fusing |
| CN109692964A (en) * | 2019-01-31 | 2019-04-30 | 中南大学 | A kind of reinforced aluminum matrix composites and preparation method thereof |
| CN111822722A (en) * | 2020-06-30 | 2020-10-27 | 长沙新材料产业研究院有限公司 | TiAl/TiB for additive manufacturing2Method for preparing powder material |
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| CN116237542A (en) * | 2023-03-15 | 2023-06-09 | 山东大学 | In-situ generation and non-original addition method, material and application of reinforcing phase of GH3230 |
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