CN109599479A - A kind of thermoelectric material and preparation method thereof - Google Patents
A kind of thermoelectric material and preparation method thereof Download PDFInfo
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- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
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Abstract
The invention discloses a kind of thermoelectric material and preparation method thereof, the preparation method is the following steps are included: take or prepare the thermoelectric material powder for meeting 3D printing Particle size requirements;Adhesive powder is dissolved in solvent, semisolid binder is made;The above thermoelectric material powder is then added, mixes, thermoelectricity slurry is made;3D printing is carried out using fusion sediment technology, thermoelectric material is made;It is dried again, sintering processes.Thermoelectric material is prepared by above method, production cost is low, and with short production cycle, waste of material is few, can print the block thermoelectric material of arbitrary shape, and obtained thermoelectric material thermal conductivity is low.
Description
Technical field
The present invention relates to thermoelectric material preparation technical fields, and in particular to a kind of thermoelectric material and preparation method thereof.
Background technique
Thermoelectric material, which refers to, realizes thermal energy and electric energy using the Seebeck effect of material, paltie effect and thomson effect
A kind of material mutually converted.By thermoelectric material prepare thermo-electric device, due to its with no mechanical moving element, it is noiseless,
The advantage of the uniqueness such as high reliability has broad application prospects in fields such as electronics.In today's society, with energy shortage and
Environmental problem is got worse, this makes a kind of extensive pass of the thermoelectric material as new energy material by industry and academia
Note.
Traditional thermoelectric material preparation method includes block cutting, powder hot-pressing, discharge plasma sintering etc., these are all
It is the process for subtracting material manufacture.These preparation methods not only complex process, preparation cost is high, and waste of raw materials is serious, prepared
Material shape is also restricted, and can only prepare the block materials of specific shape.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of preparation methods of thermoelectric material, to improve Conventional thermoelectric
The problem of block materials of specific shape can only be prepared in material processing.
The technical scheme adopted by the invention is that: a kind of preparation method of thermoelectric material, comprising the following steps:
S1, take or prepare the thermoelectric material powder for meeting 3D printing Particle size requirements;
S2, adhesive powder is dissolved in solvent, semisolid binder is made;
S3, the thermoelectric material powder is added in the resulting semisolid binder of step S2, mixing, thermoelectricity slurry is made
Material;
S4,3D printing is carried out using fusion sediment technology, thermoelectric material is made;
S5, the thermoelectric material is dried, obtains dry block thermoelectric material;Then it is sintered.
The operation order of above step S1 and step S2 also interchangeable.
In step S1, ball-milling treatment is carried out to thermoelectric material powder using ball-milling technology, until powder body material reaches micron
The order of magnitude;Then the good powder body material of ball milling is sieved, to obtain the thermoelectric material powder that can meet 3D printing Particle size requirements.Its
In, thermoelectric material powder can be p-type or N-type thermoelectric material powder.1000~1500 mesh screens can be used in the sieve of sieving processing,
It is preferred that the partial size of the thermoelectric material powder is less than 13 μm.The specific process parameter of ball-milling treatment is preferred are as follows: in inert gas ring
In border, 3~12h of ball milling under 300~500rpm revolving speed is milled to particle of the resulting powder body material partial size between 1~12 μm
Account for 90% or more of sum;Wherein, inert gas includes nitrogen, helium, argon gas, neon, xenon etc..
Preferably, in step S2, the binder is generally organic binder, specifically may include polylactic acid (PLA), poly- second
At least one of enol (PVA), polyvinylpyrrolidone (PVP), polyethylene glycol oxide (PEO) and Kynoar (PVDF).
Solvent is usually volatile solvent, and water, alcohol and dimethylformamide (DMF) etc. specifically can be used.Binder and solvent are preferred
Mix by following weight percent: the mass fraction of binder is 1~15%, and the mass fraction of solvent is 85~99%;Two
In person's mixed process, it can make binder uniform dissolution in solvent by mechanical stirring, to form semisolid binder.
Preferably, thermoelectricity slurry obtained by step S3 has following rheologic behavio(u)r: when being not pressurized, the thermoelectricity slurry
The elasticity modulus of material is greater than loss modulus;When there is pressure, the elasticity modulus of the thermoelectricity slurry is less than loss modulus.The rheology
Performance is usually formed with the raw material of thermoelectricity slurry and the factors such as proportion are related.Thermoelectric material powder and semisolid binder are preferred
Mix by following weight percent: the mass fraction of thermoelectric material powder is 60~90%, the mass fraction of semisolid binder
It is 10~40%.Thermoelectric material powder is set to be evenly distributed on half by mechanical stirring using mixing platform in the two mixed process
In solid-state adhesion agent, the thermoelectricity slurry of stable homogeneous is formed;The mixing speed of mixing platform preferably 1000~2000rpm/min, is stirred
Mix time preferably 2~5h.
Step S4 is specific can include: thermoelectricity slurry is packed into 3D printer syringe;By adjusting the pressure applied when printing
Power and print speed, so that thermoelectricity slurry can be from the smooth outflow of syringe needle;Print path is set again, so that the thermoelectricity that syringe needle squeezes out
Slurry is formed on stamp pad by preset print path.Wherein it is preferred to which applying pressure is 20~100psi, print speed
For 1~30mm/s;The print path monolayer material that concretely broken line prints that monolayer material or broken line print back and forth back and forth is folded
Addition multilayer material.In addition, the preferred diameter of the syringe needle of printer is 50~500 μm, can print out directly using the syringe needle of the diameter
Diameter is 50~500 μm, the arbitrary block thermoelectric material of length.
In step s 5, it is dried the thermoelectric material after the completion of printing can be specifically placed in baking oven and be dried,
Preferably 50~70 DEG C of drying temperature, time preferably 10~20h ultimately forms dry heat so that solvent therein sufficiently volatilizees
Electric material.In addition, specifically the thermoelectric material after drying can be placed in high temperature when being sintered to the thermoelectric material after drying
It is sintered in tube furnace, so that organic binder decomposes removal some or all of in thermoelectric material, to reduce organic binder shadow
Ring conductivity.Preferably, sintering atmosphere is inert gas (such as nitrogen, helium, neon, argon gas, argon gas, xenon) environment, is burnt
Junction temperature is 100~450 DEG C, and sintering time is 1~8h.Due to the decomposition of sintering process binder, formed in thermoelectric material thin
Small micropore, in addition, thermoelectric material is usually still partial organic substances residual after sintering, so as to make final block thermoelectricity obtained
Material has lower thermal conductivity.
The present invention also provides a kind of thermoelectric materials, are made by the preparation method of any of the above thermoelectric material.
The method have the benefit that: the present invention provides a kind of thermoelectric material and preparation method thereof, the preparation method
By first preparing thermoelectricity slurry, fusion sediment technology is recycled to carry out 3D printing to configured thermoelectricity slurry, so as to basis
Printing path is arranged to produce the block thermoelectric material of required shape in demand.Thermoelectric material is prepared by this method, is produced into
This is low, and with short production cycle, waste of material is few, can print the block thermoelectric material of arbitrary shape.The block heat of conventional method preparation
The thermal conductivity of electric material is generally higher than 0.8W/ (mK), and the block thermoelectric material relative to conventional method preparation, institute of the present invention
The thermoelectric material of preparation has the characteristics that thermal conductivity is low, and thermal conductivity is generally less than 0.6W/ (mK).
Detailed description of the invention
For the clearer technical solution illustrated in the embodiment of the present invention, will make below to required in embodiment description
Attached drawing briefly describes.
Fig. 1 is the schematic diagram for carrying out 3D printing in embodiment 1 by default print path using fusion sediment technology.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
A kind of fusion sediment technology manufacture low-heat leads Bi0.5Sb1.5Te3The method of base thermoelectricity material, comprising the following steps:
Using ball-milling technology by Bi0.5Sb1.5Te3The partial size of thermoelectric material powder is milled to a micron order of magnitude, specific ball milling
When technological parameter are as follows: in an argon atmosphere, ball milling 10h under the revolving speed of 400rpm is milled to resulting powder body material partial size 1
Particle between~12 μm accounts for 90% or more of sum.
By the good Bi of ball milling0.5Sb1.5Te3Thermoelectric material powder crosses 1000 meshes.
Polylactic acid (PLA) adhesive powder is dissolved in aqueous solvent, the mass fraction of polylactic acid is 10%, the quality point of water
Number is 90%, and stirring dissolves its substantially uniformity, forms the binder of semisolid;
By Bi0.5Sb1.5Te3Thermoelectric material powder is added in the binder of semisolid, Bi0.5Sb1.5Te3Mass fraction be
80%, the mass fraction of the binder of semisolid is 20%, is stirred using mixing platform, and the stirring rate of mixing platform is 2000rpm/
Min, mixing time 5h form the heat of stable homogeneous so that thermoelectric material powder is evenly distributed in the binder of semisolid
Plasma-based material;
Test b i0.5Sb1.5Te3The rheologic behavio(u)r of thermoelectricity slurry (is being not added when it meets specific rheologic behavio(u)r
Elasticity modulus is greater than loss modulus when pressure, and elasticity modulus is less than loss modulus when having pressure) when, it is straight that thermoelectricity slurry is packed into syringe needle
In the syringe that diameter is 100 μm, prepare to carry out 3D printing using fusion sediment technology;
The pressure and print speed that apply when adjusting printing, applications pressure are 50psi, print speed 15mm/s, so that
Thermoelectricity slurry can be smooth from syringe needle outflow;
Print path is set, and print path is that broken line prints monolayer material, forward travel distance 1cm back and forth, and line-to-line is divided into
95 μm, broken line prints back and forth, as shown in Figure 1, forming the thermoelectricity slurry 2 squeezed out from syringe needle 1 on stamp pad, block is made
Body heat electric material;
Resulting block thermoelectric material will be printed to place in an oven a period of time, oven temperature is 50 DEG C, drying time
Dry block thermoelectric material is eventually become so that the aqueous solvent in thermoelectricity slurry is sufficiently volatilized for 10h;
Block thermoelectric material is subjected to subsequent heat treatment, specifically places it in high temperature process furnances and is sintered, sintering atmosphere is
Nitrogen, sintering temperature are 450 DEG C, sintering time 6h, so that the partial organic substances in block thermoelectric material are decomposed, are ultimately formed
The block thermoelectric material that low-heat is led.
Embodiment 2
A kind of method that fusion sediment technology manufacture low-heat leads PEDOT:PSS base thermoelectricity material, comprising the following steps:
The partial size of PEDOT:PSS powder thermoelectric material is milled to a micron order of magnitude using ball-milling technology, work when ball milling
Skill parameter are as follows: in an argon atmosphere, ball milling 3h under the revolving speed of 450rpm, the resulting powder body material partial size of ball milling 1~10 μm it
Between particle account for sum 90% or more.
The good PEDOT:PSS thermoelectricity powder body material of ball milling is crossed into 1500 meshes.
Polyvinylpyrrolidone (PVP) adhesive powder is dissolved in solvent dimethylformamide (DMF), polyvinyl pyrrole
The mass fraction of alkanone is 10%, and the mass fraction of dimethylformamide is 90%, and stirring dissolves its substantially uniformity, forms half
Solid binder;
PEDOT:PSS thermoelectric material powder is added in the binder of semisolid, the mass fraction of PEDOT:PSS is
75%, the mass fraction of the binder of semisolid is 25%, is stirred using mixing platform, and the stirring rate of mixing platform is 1500rpm/
Min, mixing time 4h form the heat of stable homogeneous so that thermoelectricity powder body material is evenly distributed in the binder of semisolid
Plasma-based material;
The rheologic behavio(u)r for testing PEDOT:PSS thermoelectricity slurry, (is being not pressurized when it meets specific rheologic behavio(u)r
When elasticity modulus be greater than loss modulus, when having pressure elasticity modulus be less than loss modulus) when, by thermoelectricity slurry be packed into needle diameter
In 200 μm of syringes, to prepare to carry out 3D printing using fusion sediment technology;
The pressure and print speed that apply when adjusting printing, applications pressure are 40psi, print speed 20mm/s, so that
Thermoelectricity slurry can be smooth from syringe needle outflow;
Print path is set, and print path is that broken line prints monolayer material, forward travel distance 1cm back and forth, and line-to-line is divided into
190 μm, broken line prints back and forth, so that forming on stamp pad from the thermoelectricity slurry squeezed out in syringe needle, block thermoelectric material is made;
Resulting thermoelectric block body material will be printed to place in an oven a period of time, oven temperature is 55 DEG C, drying time
Dry thermoelectric block body material is eventually become so that the solvent dimethylformamide (DMF) in thermoelectricity slurry sufficiently volatilizees for 15h
Material;
Block thermoelectric material is subjected to subsequent heat treatment, specifically places it in high temperature process furnances and is sintered, sintering atmosphere is
Nitrogen, sintering temperature are 100 DEG C, sintering time 8h, so that the partial organic substances in block thermoelectric material are decomposed, are ultimately formed
The thermoelectric material that low-heat is led.
Above embodiments 1 and embodiment 2 recycle fusion sediment technology to configured heat by first configuring thermoelectricity slurry
Plasma-based material carries out 3D printing, so as to printing path be arranged according to demand to produce the block thermoelectric material of required shape.It is logical
It crosses this method and prepares thermoelectric material, production cost is low, and with short production cycle, waste of material is few, can print the block heat of arbitrary shape
Electric material, and prepared thermoelectric material has the characteristics that thermal conductivity is low.The thermoelectric material prepared using fusion sediment technology,
Thermal conductivity is generally less than 0.6Wm-1K-1, and the thermoelectric material thermal conductivity of traditional method preparation is generally higher than 0.8Wm-1K-1.Thermal conductivity
Rate is all made of laser conductometer and synchronous solving measures.
Although specifically showing and describing the present invention in conjunction with preferred embodiment, those skilled in the art should be bright
It is white, it is not departing from the spirit and scope of the present invention defined by described claims, it in the form and details can be right
The present invention makes a variety of changes, and is protection scope of the present invention.
Claims (10)
1. a kind of preparation method of thermoelectric material, which comprises the following steps:
S1, take or prepare the thermoelectric material powder for meeting 3D printing Particle size requirements;
S2, adhesive powder is dissolved in solvent, semisolid binder is made;
S3, the thermoelectric material powder is added in the resulting semisolid binder of step S2, thermoelectricity slurry is made in mixing;
S4,3D printing is carried out using fusion sediment technology, thermoelectric material is made;
S5, the thermoelectric material is dried, obtains dry thermoelectric material;Then it is sintered;
Step S1 and step S2 can be exchanged.
2. the preparation method of thermoelectric material according to claim 1, which is characterized in that in step S1, the thermoelectric material
The partial size of powder is less than 13 μm.
3. the preparation method of thermoelectric material according to claim 1, which is characterized in that in step S3, the thermoelectricity slurry
With following rheologic behavio(u)r: when being not pressurized, the elasticity modulus of the thermoelectricity slurry is greater than loss modulus;When there is pressure,
The elasticity modulus of the thermoelectricity slurry is less than loss modulus.
4. the preparation method of thermoelectric material according to any one of claim 1-3, which is characterized in that in step S2, institute
Stating binder includes at least one in polylactic acid, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol oxide and Kynoar
Kind.
5. the preparation method of thermoelectric material according to claim 4, which is characterized in that in the semisolid binder, institute
The mass fraction for stating binder is 1~15%, and the mass fraction of the solvent is 85~99%.
6. the preparation method of thermoelectric material according to claim 5, which is characterized in that in the thermoelectricity slurry, the heat
The mass fraction of electric material powder is 60~90%, and the mass fraction of the semisolid binder is 10~40%.
7. the preparation method of thermoelectric material according to any one of claim 1-3, which is characterized in that in step S4, institute
3D printing process is stated, application pressure is 20~100psi, and print speed is 1~30mm/s.
8. the preparation method of thermoelectric material according to claim 7, which is characterized in that the 3D printing process, print path
Line prints the monolayer material that monolayer material or broken line print back and forth for broken line back and forth and is superimposed as multilayer material.
9. the preparation method of thermoelectric material according to any one of claim 1-3, which is characterized in that in step s 5,
The temperature of the drying process is 50~70 DEG C, and the time is 10~20h;Sintering atmosphere is inert gas environment, and sintering temperature is
100~450 DEG C, sintering time is 1~8h.
10. a kind of thermoelectric material, which is characterized in that the preparation method system of the thermoelectric material as described in any one of claim 1-9
?.
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CN110171129A (en) * | 2019-05-30 | 2019-08-27 | 上海应用技术大学 | A kind of preparation method of layered polymer base composite thermoelectric material |
CN110729391A (en) * | 2019-07-30 | 2020-01-24 | 上海彩石激光科技有限公司 | Method and device for preparing magnesium silicide thermoelectric material block and thermoelectric material block |
CN110783448A (en) * | 2019-07-30 | 2020-02-11 | 武汉理工大学 | Method for manufacturing micro thermoelectric device based on femtosecond laser technology |
CN114535601A (en) * | 2022-01-24 | 2022-05-27 | 武汉理工大学 | Scraping-free method for printing thermoelectric material by selective laser melting process and scraping-free method for taking thermoelectric powder as printing raw material |
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CN110783448A (en) * | 2019-07-30 | 2020-02-11 | 武汉理工大学 | Method for manufacturing micro thermoelectric device based on femtosecond laser technology |
CN110783448B (en) * | 2019-07-30 | 2020-10-16 | 武汉理工大学 | Method for manufacturing micro thermoelectric device based on femtosecond laser technology |
CN110729391B (en) * | 2019-07-30 | 2023-09-19 | 上海彩石激光科技有限公司 | Method and device for preparing magnesium silicide thermoelectric material block and thermoelectric material block |
CN114535601A (en) * | 2022-01-24 | 2022-05-27 | 武汉理工大学 | Scraping-free method for printing thermoelectric material by selective laser melting process and scraping-free method for taking thermoelectric powder as printing raw material |
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