CN107020388A - A kind of preparation method of 3D printing TiAl intermetallic compound powder - Google Patents

A kind of preparation method of 3D printing TiAl intermetallic compound powder Download PDF

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Publication number
CN107020388A
CN107020388A CN201611266313.7A CN201611266313A CN107020388A CN 107020388 A CN107020388 A CN 107020388A CN 201611266313 A CN201611266313 A CN 201611266313A CN 107020388 A CN107020388 A CN 107020388A
Authority
CN
China
Prior art keywords
method described
intermetallic compound
reducing agent
compound powder
tial intermetallic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201611266313.7A
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Chinese (zh)
Inventor
张建勋
韩昶
候晓翠
张龙
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Qingdao Apulse Intellectual Property Management Co Ltd
QINGDAO R & D INSTITUTE XI'AN JIAOTONG UNIVERSITY
Original Assignee
Qingdao Apulse Intellectual Property Management Co Ltd
QINGDAO R & D INSTITUTE XI'AN JIAOTONG UNIVERSITY
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Application filed by Qingdao Apulse Intellectual Property Management Co Ltd, QINGDAO R & D INSTITUTE XI'AN JIAOTONG UNIVERSITY filed Critical Qingdao Apulse Intellectual Property Management Co Ltd
Priority to CN201611266313.7A priority Critical patent/CN107020388A/en
Publication of CN107020388A publication Critical patent/CN107020388A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00Materials specially adapted for additive manufacturing

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses a kind of preparation method of 3D printing with TiAl intermetallic compound powder, including selecting suitable titanium salt and aluminium salt, adjust and reduced after PH, the second reducing agent Reduced separating again is used after centrifugation, powder component produced by the present invention is uniform, epigranular, while secondary reduction method, and by the way of the different reducing agent of reducing power, it is to avoid the particle diameter of first reduction is big, the problem of easily reunite, while improve the recovery rate of powder.

Description

A kind of preparation method of 3D printing TiAl intermetallic compound powder
Technical field
The invention belongs to materials processing technology field, more particularly, to a kind of 3D printing TiAl intermetallic compound powder Preparation method.
Background technology
Titanium aluminum binary series intermetallic compound, density is smaller, in compound in addition to metallic bond, also with covalent bond, Thus it is referred to as intermetallic compound, thus intensity, hardness are big, resistance to elevated temperatures is strong, its corrosion resistance and crocking resistance Common titanium alloy, especially γ bases TiAl intermetallic compound are above because with high specific strength, high specific stiffness, anti-corrosion, resistance to The advantages of mill, high temperature resistant and excellent antioxygenic property, as fields such as contemporary aerospace industry, civilian industries One of good candidates structural material, particularly has broad application prospects in blade of aviation engine field.Current aviation hair Motivation blade is generally casting or forging method shaping, and 3D printing, or increasing material manufacturing are quick as one kind of rising in recent years Moulding process, using successively powdering, laser or electron beam melt the mode being molded, and realize the finishing shaping of precise part, And the defects such as the shrinkage cavity shrinkage porosity of casting process appearance are avoided, as a kind of emerging material manufacturing process.For 3D printing For, the parameter such as purity, granularity of powder directly affects the material property after shaping, thus the preparation method and powder of research powder The performance of material has great importance.But not yet find to prepare the 3D of TiAl-base alloy workpiece and correlation using 3D printing at present The report of printing TiAl intermetallic compound powder, preparation method thereof used.
The content of the invention
In order to solve the above technical problems, the invention provides preparation method of the 3D printing with TiAl intermetallic compound powder, By the way of chemical reduction method secondary reduction, the recovery rate of powder is improved, and improves the uniformity of powder particles.
The complete technical scheme of the present invention includes:
The preparation method of a kind of 3D printing TiAl intermetallic compound powder, it is characterised in that comprise the following steps:
1) titanium salt solution that selection concentration is 0.1-0.13mol/L, and 0.1-0.13mol/L aluminum salt solution are mixed, plus Enter ultrasonic wave under cationic surfactant mixed liquor, heating condition to stir;
2) ammoniacal liquor regulation pH value is added;
3) the first reducing agent, the lower heating response of ultrasonic wave stirring are added;
4) reaction solution is centrifuged, sediment washing is dried to obtain first group of TiAl intermetallic compound powder product;
5) the second reducing agent, the lower heating response of ultrasonic wave stirring will after the supernatant concentration after centrifugation, be added;
6) reaction solution is centrifuged, sediment washing is dried to obtain second group of TiAl intermetallic compound powder product.
It is preferred that, first reducing agent and the second reducing agent reducing power are different.
It is preferred that, cationic surfactant be volume ratio be chlorination benzalkonium, lauryl dimethyl benzyl ammonium chloride, C15The mixture of trimethylammonium bromide.
It is preferred that, step 2) in ammoniacal liquor regulation pH value be 5-9.
It is preferred that, reducing agent adds the 1/4-1/6 that volume is mixeding liquid volume.
It is preferred that, step 1) in heating-up temperature be 40-60 DEG C.
It is preferred that, step 5) in heating-up temperature be 120-160 DEG C.
The present invention is relative to the advantage of prior art:Traditionally, the processing side that powder metallurgy etc. is molded using powder Powder used in method includes two kinds of alloyed powder and element powder, and carries out institute in forming method using TiAl intermetallic compound powder at present Powder is typically to select the Ti alloyed powders and Al alloyed powders that meet proportioning to be reprocessed after being mixed in processing, process not It is evitable to there is uneven, the problems such as deviation occurs in local component of mixing, and the present invention uses chemical combination reducing process, directly makes Standby to go out to meet the TiAl intermetallic compound powder of component requirements, powder component is uniform, and printing effect is improved during 3D printing Fruit and component capabilities, while designing chemical reduction method preparation technology prepared by suitable TiAl intermetallic compound powder, are obtained Powder Particle Size is uniform, while secondary reduction method, and by the way of the different reducing agent of reducing power, it is to avoid the grain of first reduction Footpath is big, the problem of easily reunite, while improving the recovery rate of powder.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1:
The preparation method of a kind of 3D printing TiAl intermetallic compound powder, it is characterised in that comprise the following steps:
1) by 0.25mol TiCl42L deionized waters are dissolved in, TiCl is configured to4The aqueous solution, by 0.22mol AlCl3 1.78L deionized waters are dissolved in, AlCl is configured to3The aqueous solution, both are mixed, and are added cationic surfactant and are mixed Liquid A, cationic surfactant is that volume ratio is chlorination benzalkonium:Lauryl dimethyl benzyl ammonium chloride:C15Front three bromide Change ammonium=1:2:1 mixture, is heated to 40-60 DEG C and ultrasonic wave stirring 5-10min is standby;
2) mixed liquid B is obtained toward adding ammoniacal liquor in previous solu and adjust its PH for 8.5;
3) it is 0.1mol/L glucose and the mixture of formaldehyde that total moles quality, which is added dropwise, and addition volume is mixed liquor The 1/4-1/6 of B volumes, obtains mixed liquor C, and heating-up temperature reacts 10-15min to 80-120 DEG C under the conditions of ultrasonic agitation;
4) reacted mixture C is centrifuged 10 minutes with 5000rpm rotating speed, the sediment after separation is spent Ion water washing 3-4 times, it is slow at 100-120 DEG C to dry 30min, obtain first group of TiAl intermetallic compound powder product;
5) by step 4) centrifuge after obtained supernatant liquor be concentrated into the 1/3-1/2 of original volumes, obtain mixed liquor D, is subsequently added ascorbic acid and hydrazine hydrate mixture that total moles quality is 0.12mol/L, and addition volume is mixed liquor D volumes 1/4-1/6, be subsequently heated temperature for 120-160 DEG C, 10-15min reacted under the conditions of ultrasonic agitation;
6) mixture is centrifuged 10 minutes with 5000rpm rotating speed, by the sediment deionization after separation Water washing 3-4 times, it is slow at 100-120 DEG C to dry 30min, obtain second group of TiAl intermetallic compound powder product.
Embodiment 2:
Using the chloride in Ti and Al nitrate substitution embodiment 1, while being replaced using anion surfactant Cationic surfactant, other technological parameters are same as Example 1.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, it is every according to the present invention Any simple modification, change and equivalent structure change that technical spirit is made to above example, still fall within skill of the present invention In the protection domain of art scheme.

Claims (8)

1. a kind of 3D printing preparation method of TiAl intermetallic compound powder, it is characterised in that comprise the following steps:
1) titanium salt solution that selection concentration is 0.1-0.13mol/L, and 0.1-0.13mol/L aluminum salt solution are mixed, and add sun Ultrasonic wave is stirred under ionic surface active agent mixed liquor, heating condition;
2) ammoniacal liquor regulation pH value is added;
3) the first reducing agent, the lower heating response of ultrasonic wave stirring are added;
4) reaction solution is centrifuged, sediment washing is dried to obtain first group of TiAl intermetallic compound powder product;
5) the second reducing agent, the lower heating response of ultrasonic wave stirring will after the supernatant concentration after centrifugation, be added;
6) reaction solution is centrifuged, sediment washing is dried to obtain second group of TiAl intermetallic compound powder product.
2. the method described in claim 1, it is characterised in that first reducing agent and the second reducing agent reducing power are different.
3. the method described in claim 2, it is characterised in that cationic surfactant be volume ratio be chlorination benzalkonium, Lauryl dimethyl benzyl ammonium chloride, C15The mixture of trimethylammonium bromide.
4. the method described in claim 4, it is characterised in that step 2) in ammoniacal liquor regulation pH value be 5-9.
5. the method described in claim 4, it is characterised in that reducing agent adds the 1/4-1/6 that volume is mixeding liquid volume.
6. the method described in claim 5, it is characterised in that step 1) in heating-up temperature be 40-60 DEG C.
7. the method described in claim 6, it is characterised in that step 5) in heating-up temperature be 120-160 DEG C.
8. the method described in claim 7, it is characterised in that the titanium salt and aluminium salt are nitrate or chloride.
CN201611266313.7A 2016-12-31 2016-12-31 A kind of preparation method of 3D printing TiAl intermetallic compound powder Pending CN107020388A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611266313.7A CN107020388A (en) 2016-12-31 2016-12-31 A kind of preparation method of 3D printing TiAl intermetallic compound powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611266313.7A CN107020388A (en) 2016-12-31 2016-12-31 A kind of preparation method of 3D printing TiAl intermetallic compound powder

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CN107020388A true CN107020388A (en) 2017-08-08

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106825603A (en) * 2016-12-31 2017-06-13 西安交通大学青岛研究院 A kind of aluminium coats the preparation method of titanium composite alloy powder

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106825603A (en) * 2016-12-31 2017-06-13 西安交通大学青岛研究院 A kind of aluminium coats the preparation method of titanium composite alloy powder

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Application publication date: 20170808