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 PDFInfo
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- 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
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- Prior art keywords
- method described
- intermetallic compound
- reducing agent
- compound powder
- tial intermetallic
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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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE 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
- B33Y70/00—Materials specially adapted for additive manufacturing
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- 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
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.
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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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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 |