CN109112362A - A kind of dedicated substrate of Ti-Ni marmem and preparation method thereof of 4D printing flawless - Google Patents
A kind of dedicated substrate of Ti-Ni marmem and preparation method thereof of 4D printing flawless Download PDFInfo
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- CN109112362A CN109112362A CN201811004388.7A CN201811004388A CN109112362A CN 109112362 A CN109112362 A CN 109112362A CN 201811004388 A CN201811004388 A CN 201811004388A CN 109112362 A CN109112362 A CN 109112362A
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- marmem
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
-
- 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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- 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0433—Nickel- or cobalt-based alloys
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- Mechanical Engineering (AREA)
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Abstract
The invention discloses a kind of dedicated substrates of Ti-Ni marmem and preparation method thereof of 4D printing flawless, the substrate is made of Ni, Ti, Zr, by percentage to the quality, the Ni content is 40%~80%, the Ti content is 10%~60%, the Zr content is 2~10%.The dedicated substrate of the 4D printing Ti-Ni marmem of flawless has been prepared in the present invention, and substrate hardness prepared by the present invention and intensity are high, good toughness, not easy to crack.
Description
Technical field
The invention belongs to alloy preparation and increases material manufacturing technology fields, and in particular to a kind of titanium nickel shape of 4D printing flawless
Dedicated substrate of shape memory alloys and preparation method thereof.
Background technique
Ti-Ni marmem is the memorial alloy developed earliest, since exploitation in 1963, due to its memory effect
Answer excellent, performance is stable, good biocompatibility and receive the extensive attention of material science and engineering circles.Since titanium nickel shape is remembered
Recall the processing cost height of alloy and preparation processing technology is complicated, limits it in the application in many fields.It is asked to solve these
Topic, needs researchers constantly to develop new preparation process.The existing method for preparing Ti-Ni marmem
Totally five kinds other than SLM: smelting process, powder metallurgic method, discharge sintering method, Ti-Ni marmem sputtering method and from climing
Prolong high-temperature synthesis.These methods have the shortcomings that common: can not prepare complex-shaped workpiece.SLM technology is to utilize metal
Powder is completely melt under the heat effect of laser beam, molding a kind of increasing material (Additive through cooled and solidified
Manufacturing) technology.For selective laser melting process for conventional method, the sample dimensional accuracy of preparation is higher,
And it is capable of processing the part with complex shape that conventional method is not capable of processing.SLM, which prepares Ti-Ni marmem needs, to be made
It is easily cracked with the titanium ni substrate of the titanium ni substrate of same composition, but the preparation of existing process, influences its use
Performance.
How to prepare the dedicated substrate of the Ti-Ni marmem of the 4D printing of flawless is the key that this technology.
Summary of the invention
The purpose of this section is to summarize some aspects of the embodiment of the present invention and briefly introduce some preferable implementations
Example.It may do a little simplified or be omitted to avoid our department is made in this section and the description of the application and the title of the invention
Point, the purpose of abstract of description and denomination of invention it is fuzzy, and this simplification or omit and cannot be used for limiting the scope of the invention.
In view of above-mentioned technological deficiency, the present invention is proposed.
Therefore, as one aspect of the present invention, the present invention overcomes the deficiencies in the prior art, provides a kind of 4D
Print the dedicated substrate of the Ti-Ni marmem of flawless.
In order to solve the above technical problems, the present invention provides the following technical scheme that a kind of titanium nickel shape of 4D printing flawless
The dedicated substrate of shape memory alloys, in which: the substrate is made of Ni, Ti, Zr, and by percentage to the quality, the Ni content is
40%~80%, the Ti content is 10%~60%, the Zr content is 2~10%.
A kind of preferred side of the dedicated substrate of Ti-Ni marmem as 4D of the present invention printing flawless
Case: by percentage to the quality, the Ni content is 50%~70%, the Ti content is 20%~50%, the Zr content is 2
~6%.
A kind of preferred side of the dedicated substrate of Ti-Ni marmem as 4D of the present invention printing flawless
Case: the weight percent of its each component is as follows: Ni:60%, Ti:37%, Zr:3%.
As another aspect of the present invention, the present invention overcomes the deficiencies in the prior art, provides the 4D printing
The preparation method of the dedicated substrate of the Ti-Ni marmem of flawless.
In order to solve the above technical problems, the present invention provides the following technical scheme that the titanium nickel shape of 4D printing flawless
The preparation method of the dedicated substrate of shape memory alloys comprising,
Ni powder, Ti powder and Zr powder are mixed, and the polyvinyl alcohol adhesive that 1~5wt% is added is sufficiently mixed；
By Ni, Ti, Zr mixed-powder according to 100~500 tons of pressure compression moulding；
By Ni, Ti, Zr mixed-powder vacuum-sintering at plate.
The preparation method of the dedicated substrate of Ti-Ni marmem as 4D of the present invention printing flawless
A kind of preferred embodiment: the Ni powder is the pure Ni powder of nanoscale, the Ti powder is the pure Ti powder of nanoscale, the Zr powder is that nanoscale is pure
Zr powder.
The preparation method of the dedicated substrate of Ti-Ni marmem as 4D of the present invention printing flawless
A kind of preferred embodiment: the vacuum-sintering, sintering temperature are 800~1200 DEG C, and sintering time is 1~6h.
The preparation method of the dedicated substrate of Ti-Ni marmem as 4D of the present invention printing flawless
A kind of preferred embodiment: the polyvinyl alcohol mass fraction is 2wt%.
The preparation method of the dedicated substrate of Ti-Ni marmem as 4D of the present invention printing flawless
A kind of preferred embodiment: by Ni, Ti, Zr mixed-powder according to 400 tons of pressure compression moulding.
The preparation method of the dedicated substrate of Ti-Ni marmem as 4D of the present invention printing flawless
A kind of preferred embodiment: the vacuum-sintering, sintering temperature are 1100 DEG C.
The preparation method of the dedicated substrate of Ti-Ni marmem as 4D of the present invention printing flawless
A kind of preferred embodiment: the substrate surface flawless, hardness is in 280HV or more, and tensile strength is in 760Mpa or more.
Beneficial effects of the present invention: the present invention promotes Ti by addition Zr element2The precipitation of the second phase of Ni hinders crystal grain raw
It grows and has refined crystal grain.When average grain size is smaller, the number of grain boundaries in unit volume is more, and the extension needs of crackle are worn
More crystal boundaries are crossed, this makes the generation and expansion of crackle obtain very big inhibition.Meanwhile the addition of Zr improves memory and closes
The restoring force of gold, principle are that the binding force with the addition of more Zr, between atom increases, and the intensity of alloy increases accordingly,
And the yield strength of martensite is also correspondingly improved.Therefore, the 4D printing titanium nickel shape note of flawless has been prepared
Recall the dedicated substrate of alloy, and substrate hardness prepared by the present invention and intensity are high, it is good toughness, not easy to crack.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill of field, without any creative labor, it can also be obtained according to these attached drawings other
Attached drawing.Wherein:
Fig. 1 is the substrate figure after machine-shaping of the present invention.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, right combined with specific embodiments below
A specific embodiment of the invention is described in detail.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, but the present invention can be with
Implemented using other than the one described here other way, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by the specific embodiments disclosed below.
Secondly, " one embodiment " or " embodiment " referred to herein, which refers to, may be included at least one realization side of the invention
A particular feature, structure, or characteristic in formula." in one embodiment " that different places occur in the present specification not refers both to
The same embodiment, nor the individual or selective embodiment mutually exclusive with other embodiments.
Embodiment 1:
The dedicated substrate of the 4D printing Ti-Ni marmem of flawless, the weight percent of each component are as follows: Ni:
60%, Ti:37%, Zr:3%.
The preparation method of the dedicated substrate of the 4D printing Ti-Ni marmem of flawless, includes the following steps:
The polyvinyl alcohol adhesive that the pure Ni powder of micron order, pure Ti powder and pure Zr powder are mixed, and 2wt% is added carries out abundant
Mixing；
By mixed NiTiZr powder according to 400 tons of pressure compression moulding；
It is with conventional vacuum sintering process that NiTiZr is powder sintered at plate, sintering parameter are as follows: 1100 DEG C of sintering temperature, sintering
Time 4h, and by NiTiZr sheet fabrication at the dedicated substrate of 4D printing Ti-Ni marmem.
The dedicated substrate flawless of Ti-Ni marmem, hardness are printed by the 4D that above method is prepared
280HV, tensile strength 760MPa.
Embodiment 2:
The dedicated substrate of the 4D printing Ti-Ni marmem of flawless, the weight percent of each component are as follows: Ni:
60%, Ti:38%, Zr:2%.
The preparation method of the dedicated substrate of the 4D printing Ti-Ni marmem of flawless, includes the following steps:
The polyvinyl alcohol adhesive that the pure Ni powder of micron order, pure Ti powder and pure Zr powder are mixed, and 1wt% is added carries out abundant
Mixing；
By mixed NiTiZr powder according to 390 tons of pressure compression moulding；
It is with conventional vacuum sintering process that NiTiZr is powder sintered at plate, sintering parameter are as follows: 1080 DEG C of sintering temperature, sintering
Time 3h, and by NiTiZr sheet fabrication at the dedicated substrate of 4D printing Ti-Ni marmem.
The dedicated substrate flawless of Ti-Ni marmem, hardness are printed by the 4D that above method is prepared
290HV, tensile strength 780MPa.
Embodiment 3:
The dedicated substrate of the 4D printing Ti-Ni marmem of flawless, the weight percent of each component are as follows: Ni:
60%, Ti:39%, Zr:1%.
The preparation method of the dedicated substrate of the 4D printing Ti-Ni marmem of flawless, includes the following steps:
The polyvinyl alcohol adhesive that the pure Ni powder of micron order, pure Ti powder and pure Zr powder are mixed, and 3wt% is added carries out abundant
Mixing；
By mixed NiTiZr powder according to 380 tons of pressure compression moulding；
It is with conventional vacuum sintering process that NiTiZr is powder sintered at plate, sintering parameter are as follows: 1060 DEG C of sintering temperature, sintering
Time 2h, and by NiTiZr sheet fabrication at the dedicated substrate of 4D printing Ti-Ni marmem.
The dedicated substrate flawless of Ti-Ni marmem, hardness are printed by the 4D that above method is prepared
295HV, tensile strength 775MPa.
Embodiment 4:
The dedicated substrate of the 4D printing Ti-Ni marmem of flawless, the weight percent of each component are as follows: Ni:
60%, Ti:36%, Zr:4%.
The preparation method of the dedicated substrate of the 4D printing Ti-Ni marmem of flawless, includes the following steps:
The polyvinyl alcohol adhesive that the pure Ni powder of micron order, pure Ti powder and pure Zr powder are mixed, and 4wt% is added carries out abundant
Mixing；
By mixed NiTiZr powder according to 410 tons of pressure compression moulding；
It is with conventional vacuum sintering process that NiTiZr is powder sintered at plate, sintering parameter are as follows: 1120 DEG C of sintering temperature, sintering
Time 5h, and by NiTiZr sheet fabrication at the dedicated substrate of 4D printing Ti-Ni marmem.
The dedicated substrate flawless of Ti-Ni marmem, hardness are printed by the 4D that above method is prepared
300HV, tensile strength 795MPa.
Embodiment 5:
The dedicated substrate of the 4D printing Ti-Ni marmem of flawless, the weight percent of each component are as follows: Ni:
60%, Ti:35%, Zr:5%.
The preparation method of the dedicated substrate of the 4D printing Ti-Ni marmem of flawless, includes the following steps:
The polyvinyl alcohol adhesive that the pure Ni powder of micron order, pure Ti powder and pure Zr powder are mixed, and 5wt% is added carries out abundant
Mixing；
By mixed NiTiZr powder according to 420 tons of pressure compression moulding；
It is with conventional vacuum sintering process that NiTiZr is powder sintered at plate, sintering parameter are as follows: 1140 DEG C of sintering temperature, sintering
Time 6h, and by NiTiZr sheet fabrication at the dedicated substrate of 4D printing Ti-Ni marmem, finished product is as shown in Figure 1.
The dedicated substrate flawless of Ti-Ni marmem, hardness are printed by the 4D that above method is prepared
305HV, tensile strength 800MPa.
Embodiment 6:
In order to study influence of the sintering temperature to 4D printing Ti-Ni marmem performance, setting sintering temperature is respectively
1000,1100,1200 and 1300 DEG C, remaining experimental procedure and parameter setting are same as Example 1.
The experimental results showed that at a lower temperature (1000 DEG C), powder particle is not combined through diffusion substantially, in conjunction with
Power is lower, largely remains starting powder and simply piles up state, and hole quantity is more, is distributed in irregular shape and size
Unevenly.With the raising of sintering temperature, powder particle combine it is even closer, pore appearance tends to be round and smooth, quantity reduce.But
The generation that excessively high sintering temperature (1300 DEG C) will lead to a large amount of liquid phases, it is unfavorable to being sintered, because excessive liquid phase will lead to burning
Certain contraction and collapsing occur for knot Product size, make sample deformation.
Embodiment 7:
The influence of Ti-Ni marmem performance is printed to 4D for research sintering time,
It is respectively 1h, 2h, 4h and 6h that sintering time, which is arranged, remaining experimental procedure and parameter setting are same as Example 1.
The experimental results showed that most of powder particle remains original simple when soaking time is less than or equal to 4h
Pile up state, the combination of powder also defective tightness, sintering also carries out incomplete, and the densification degree of sample is extremely low.Work as the time
When increasing to 6h, hole quantity is reduced, and pore-size is also reduced.It is less than or equal to the sample phase of 4h with soaking time
Than powder particle is even closer in combination.Mutual bonding and fusion between powder particle are the counterdiffusion of atom phase and infiltration
Result.
Embodiment 8:
The influence of Ti-Ni marmem performance is printed to 4D for research pressing pressure,
It is respectively 100,200,300 and 400 tons that pressing pressure, which is arranged, remaining experimental procedure and parameter setting are and embodiment
1 is identical.
The experimental results showed that being easy to produce more porous, induction crackle generation when pressing pressure too small (≤200 tons)；And
Pressure too big (400 tons) when, be easy to produce internal stress in substrate, improve the formation rate of crackle.When pressing pressure is 300 tons
When, substrate performance reaches best.
Embodiment 9:
In order to study metallic element to 4D printing Ti-Ni marmem substrate performance influence, be respectively adopted NiTi,
NiTiHf, NiTiNb, NiTiSc and NiTiZr are tested, and are found through experiments that, NiTi, NiTiHf, NiTiNb and NiTiSc
Occur influencing the service performance of substrate compared with multiple cracks on substrate, and without any crackle on NiTiZr substrate, service performance is good
It is good.
As one aspect of the present invention, the present invention is eliminated by the content of optimization polyvinyl alcohol, compacting and sintering parameter
The crackle of substrate, improves its service performance.For polyvinyl alcohol, the very few bond effect that will lead to of content is poor, powder
Between combination it is weak, be easy to produce crackle；Content excessively then will lead to the generation of big particle agglomerate, also will increase crackle appearance
Probability.For pressing pressure, when pressing pressure is too small, it is easy to produce more porous, induction crackle generation；And pressure is too
When big, it is easy to produce internal stress in substrate, improves the formation rate of crackle.For sintering temperature, when sintering temperature is too low,
Sintering neck is thinner, and powder particle is not bonded through diffusion substantially, and binding force is lower, and hole quantity is more, is also easy to produce
Crackle；And when sintering temperature is excessively high, a large amount of liquid phases generate, and cause sintered product that certain contraction respectively occurs to size, collapses,
Make sample deformation, meanwhile, increased thermal stress is also easy to generate crackle.It is therefore desirable to select optimal polyvinyl alcohol content,
Compacting and sintering parameter are to prepare the dedicated substrate that the 4D of flawless prints Ti-Ni marmem.Meanwhile the present invention passes through
It adds Zr element and promotes Ti2The precipitation of the second phase of Ni hinders grain growth and has refined crystal grain.When average grain size is smaller
When, the number of grain boundaries in unit volume is more, and the extension of crackle is needed across more crystal boundaries, this makes the generation and expansion of crackle
Exhibition has obtained very big inhibition.Meanwhile the addition of Zr improves the restoring force of memorial alloy, principle is as more Zr add
Enter, the binding force between atom increases, and the intensity of alloy increases accordingly, and the yield strength of martensite is also obtained and mentioned accordingly
It is high.Therefore, the dedicated substrate of the 4D printing Ti-Ni marmem of flawless, and base prepared by the present invention has been prepared
Plate hardness and strength are high, good toughness, not easy to crack.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferable
Embodiment describes the invention in detail, those skilled in the art should understand that, it can be to technology of the invention
Scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered in this hair
In bright scope of the claims.
Claims (10)
1. a kind of dedicated substrate of the Ti-Ni marmem of 4D printing flawless, it is characterised in that: the substrate by Ni,
Ti, Zr composition, by percentage to the quality, the Ni content is 40%~80%, the Ti content is 10%~60%, the Zr
Content is 2~10%.
2. the dedicated substrate of the Ti-Ni marmem of 4D printing flawless as described in claim 1, it is characterised in that: with
Mass percent meter, the Ni content is 50%~70%, the Ti content is 20%~50%, the Zr content be 2~
6%.
3. the dedicated substrate of the Ti-Ni marmem of 4D printing flawless as claimed in claim 1 or 2, feature exist
In: the weight percent of its each component is as follows: Ni:60%, Ti:37%, Zr:3%.
4. the preparation side of the dedicated substrate of the Ti-Ni marmem of any one of claims 1 to 3 4D printing flawless
Method, it is characterised in that: including,
Ni powder, Ti powder and Zr powder are mixed, and the polyvinyl alcohol adhesive that 1~5wt% is added is sufficiently mixed；
By Ni, Ti, Zr mixed-powder according to 100~500 tons of pressure compression moulding；
By Ni, Ti, Zr mixed-powder vacuum-sintering at plate.
5. the preparation method of the dedicated substrate of the Ti-Ni marmem of 4D printing flawless as claimed in claim 4,
Be characterized in that: the Ni powder is the pure Ni powder of nanoscale, the Ti powder is the pure Ti powder of nanoscale, the Zr powder is the pure Zr of nanoscale
Powder.
6. the preparation method of the dedicated substrate of the Ti-Ni marmem of 4D printing flawless as claimed in claim 4,
Be characterized in that: the vacuum-sintering, sintering temperature are 800~1200 DEG C, and sintering time is 1~6h.
7. the preparation method of the dedicated substrate of the Ti-Ni marmem of 4D printing flawless as claimed in claim 4,
Be characterized in that: the polyvinyl alcohol mass fraction is 2wt%.
8. the preparation method of the dedicated substrate of the Ti-Ni marmem of 4D printing flawless as claimed in claim 4,
It is characterized in that: by Ni, Ti, Zr mixed-powder according to 400 tons of pressure compression moulding.
9. the preparation method of the dedicated substrate of the Ti-Ni marmem of 4D printing flawless as claimed in claim 6,
Be characterized in that: the vacuum-sintering, sintering temperature are 1100 DEG C.
10. the preparation method of the dedicated substrate of the Ti-Ni marmem of 4D printing flawless as claimed in claim 4,
Be characterized in that: the substrate surface flawless, hardness is in 280HV or more, and tensile strength is in 760Mpa or more.
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| CN201811004388.7A CN109112362B (en) | 2018-08-30 | 2018-08-30 | Special substrate for 4D printing of crack-free titanium-nickel shape memory alloy and preparation method thereof |
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| CN201811004388.7A CN109112362B (en) | 2018-08-30 | 2018-08-30 | Special substrate for 4D printing of crack-free titanium-nickel shape memory alloy and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110340933A (en) * | 2019-06-28 | 2019-10-18 | 华中科技大学 | A kind of intelligent bionic crawl clamping device based on 4D printing shaping |
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| US20130130112A1 (en) * | 2011-11-17 | 2013-05-23 | Byung-joo Chung | Silicon based shape memory alloy negative active material, negative active material composition including same, rechargeable lithium battery including same, and method of preparing same |
| CN105908000A (en) * | 2016-06-16 | 2016-08-31 | 华南理工大学 | Light high-strength and high-tenacity NiTi shape memory alloy composite damping material with wide temperature range and preparing method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110340933B (en) * | 2019-06-28 | 2020-08-28 | 华中科技大学 | Intelligent bionic grabbing and clamping device based on 4D printing forming |
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