CN104103750B - Preparation method of magnesium-silicon based silicon nanowire composite thermoelectric material - Google Patents
Preparation method of magnesium-silicon based silicon nanowire composite thermoelectric material Download PDFInfo
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Abstract
The invention discloses a preparation method of a magnesium-silicon based silicon nanowire composite thermoelectric material, belongs to the field of preparation of semiconductor thermoelectric materials, and specifically discloses a technical scheme including the steps of preparing a silicon nanowire by utilizing a chemical etching way, stripping the silicon nanowire through ultrasonic oscillation and mixing the silicon nanowire with magnesium-silicon based powder synchronously and uniformly, and preparing the magnesium-silicon based silicon nanowire composite thermoelectric material through electric field assisted sintering. The preparation method of the magnesium-silicon based silicon nanowire composite thermoelectric material is characterized in that the problems of twining, agglomerating and the like of the silicon nanowire in the preparation of the composite blocky material are avoided through synchronous realization of stripping and mixing of the silicon nanowire, and the composite material which achieves uniformly distributed silicon nanowire and is well combined with the base body can be prepared in the later electric field assisted sintering process. The characteristics of the preparation method are that the source of the raw material is abundant, the cost is low, the technology is simple, the easy agglomeration problem of the nanowire is solved, the nanowire of the prepared silicon nanometer composite Mg2Si material is uniform in distribution, and the heat conductivity is low. According to the invention, a method for compositely reducing the heat conductivity of the Mg2Si based thermoelectric material and improving the thermoelectric performance by using the nanowire is provided.
Description
Technical field
The preparation method of magnesium silicon substrate silicon nanowires composite thermoelectric material, belongs to semi-conductor thermoelectric material preparation field, specifically
For be to prepare silicon nanowires using chemical etching method, through sonic oscillation realize silicon nanowires peel off and its with magnesium silicon substrate powder
Body is synchronous uniformly to be mixed, and prepares the technical scheme of magnesium silicon substrate silicon nanowires composite thermoelectric material through electric field-assisted sintering.
Background technology
Thermoelectric material is the class work(realizing mutually conversion between electric energy and heat energy using pyroelectric effect (thermoelectric effect)
Can property material.Heat to electricity conversion using be solid interior carrier, have hence with the application device that thermoelectric material is made
Easily controllable, reliability is high；Movement-less part, the advantages of noiseless, in solar electrical energy generation, used heat recycles and military aviation
Application in field has obvious advantage.The performance of thermoelectric material characterizes zt=s with dimensionless thermoelectric figure of merit zt2σ t/ κ, wherein s
For Seebeck coefficient, σ be electrical conductivity, κ be thermal conductivity.Zt value is higher, and conversion efficiency of thermoelectric is higher.A kind of good thermoelectric material should
This has high electrical conductivity and low thermal conductivity.
Low-dimensional nano structure utilizes quantum confinement by optimizing thermoelectricity capability to electric, sound transport property coordinated regulation
Effect improves the density of electronic states near fermi level, thus improving seebeck coefficient while not reducing electrical conductivity；Simultaneously
Scattering process to phonon is greatly enhanced while not increasing electron scattering based on boundary scattering effect, thus reducing lattice
Thermal conductivity.Novel nano structure thermoelectric material has one-dimensional nano line and the materials such as two-dimensional nano-film, and wherein silicon nanowires has
Excellent thermoelectricity capability.Zt value is about 1 to the silicon nanowires of a diameter of 50-100nm of document report at room temperature, and it is straight to continue reduction
Footpath, zt value increases further.
mg2Si base thermoelectricity material belongs to middle temperature (500k-800k) thermoelectric material, has cheap, nontoxic, corrosion-resistant, high temperature
The good feature of stability inferior, is a kind of new green power material.With mg2Si is the solid solution of base, and effective mass is big, mobility
Greatly, lattice thermal conductivity is little, is with a wide range of applications.But simple mg2The lattice thermal conductivity of si is higher, limits its heat
The raising of electrical property.
Content of the invention
The purpose of the preparation method of magnesium silicon substrate silicon nanowires composite thermoelectric material of the present invention is: for solving above-mentioned existing skill
The problem of art, open one kind utilizes silicon nanowires and mg2Si thermoelectric material is combined and effectively reduces matrix thermal conductivity, by doping
Sb, bi, la or ag improve and optimize mg2Si sill thermoelectricity capability, synchronously realizes silicon nanowires stripping and mixing avoids silicon to receive
Rice noodles are wound around in composite block material preparation and reunite, and prepare silicon nanowire distribution in later stage electric field-assisted sintering process
The method of the magnesium silicon substrate silicon nanowires composite thermoelectric material being well combined uniformly and its with matrix, the method process is simple, finished product
Rate is high, can effectively improve the thermoelectricity capability of magnesium silicon substrate thermoelectric material, the exploitation for high performance thermoelectric material has important science
Meaning and using value.
The preparation method of magnesium silicon substrate silicon nanowires composite thermoelectric material of the present invention is it is characterised in that be a kind of using silicon nanometer
Line and mg2Si thermoelectric material is combined and effectively reduces matrix thermal conductivity, is improved by adulterate sb, bi, la or ag and optimizes mg2Si base
Conducting material thermoelectricity performance, synchronously realize silicon nanowires peel off and mixing avoid silicon nanowires composite block material preparation in be wound around and
Reunite, later stage electric field-assisted sintering process is prepared the magnesium silicon substrate that silicon nanowire distribution is uniform and its is well combined with matrix
The method of silicon nanowires composite thermoelectric material, the method is to utilize agno3Solution is etching liquid with the mixed liquor of hf acid, in monocrystalline
On silicon chip normal temperature etching 3h-4h prepare silicon nanowires, the silicon chip after etching go silver process cleaning after with purity > 99%, granularity
≤850μmmg2The absolute ethyl alcohol that the si powder and x element for sb, bi, la and ag is concurrently placed at water content ＜ 0.03wt.% is molten
Ultrasonic mixing in liquid, mixed solution drying and processing in the environment of vacuum ＞ 0.09mpa, the powder after drying is carried out
Ball milling, in order to avoid the pollution in mechanical milling process, using ball grinder and the zro of polytetrafluoroethylene (PTFE)2Abrading-ball, the powder after ball milling is put
In graphite jig, block nanometer is sintered into using fapas method and be combined hot material, whole process is as shown in figure 1, concrete steps
As follows:
1) measure agno respectively with graduated cylinder and dropper3Solution and hf acid, the two are mixed in beaker and are made into etching
Liquid 1, twin polishing monocrystalline silicon piece 2 is placed in etching liquid, etches 3-4h under normal temperature；
2) silicon chip after etching goes silver to clean 5-10min with distilled water, by the silicon cleaning up after processing in red fuming nitric acid (RFNA)
Piece 3 is placed in standby in the beaker of ethanol solution 4, the water content ＜ 0.03wt.% of ethanol solution 4；
3) weigh the mg that mole mixture ratio example is 0.96≤x≤0.99 in vacuum glove box2Si powder and bi powder, form
Mixed powder 5 is placed in solution 4；
4) beaker of solution 4 sonic oscillation 20-25min in supersonic wave cleaning machine 6 will be filled, then take out silicon chip, remain
Remaining solution 7 is placed in vacuum environment and carries out magnetic agitation and vacuum drying, vacuum ＞ on temperature control magnetic stirring apparatus 8 simultaneously
0.09mpa, drying temperature is 35 DEG C, and the time is 120min.
5) powder after drying is placed in polytetrafluoroethylene (PTFE) ball grinder ball milling 4h on planetary ball mill, ratio of grinding media to material is
8:1, forms powder 9；
6) powder 9 is placed in graphite jig 10, through 15min temperature liter in the vacuum fapas stove of vacuum ＞ 10pa
To 750 DEG C, it is incubated 20min, in insulating process, pressure is 60mpa, after insulation terminates, close electric current heating, release, sample is with stove
Cooling.
The preparation method of magnesium silicon substrate silicon nanowires composite thermoelectric material of the present invention has the beneficial effect that the silicon after etching
The silicon nanowires of the stripping that piece obtains through sonic oscillation, diameter has reached nanoscale (as shown in Figure 2).Synchronization achieves silicon line
Stripping and powder mixing, efficiently solve the easy agglomeration traits of silicon nanowires so that silicon nanowires in the base can be uniform
Distribution (as shown in Figure 3).The magnesium silicon substrate silicon nanowires composite thermoelectric material of present invention preparation, silicon nanowires can be stored in matrix material
In crystal grain, run through two to three crystal grain (as shown in Figure 4), successfully achieve the system of magnesium silicon substrate silicon nanowires composite thermoelectric material
Standby.The thermal conductivity of magnesium silica-based nanowire composite thermoelectric material is significantly lower than the thermal conductivity (as shown in Figure 5) of magnesium silica-base material.
Brief description
Fig. 1 prepares the procedure chart of magnesium silicon substrate silicon nanowires composite thermoelectric material, in figure
1- etching liquid 2- monocrystalline silicon piece 3- removes the silicon chip 4- ethanol solution 5-mg after silver cleaning2Si powder and bi powder
Powder after the mixed liquor 8- temperature control magnetic stirring apparatus 9- ball milling of 6- ultrasonic washing instrument 7- silicon nanowires, powder and absolute ethyl alcohol
Body 10- graphite jig
The free silicon nanowires sem pattern that Fig. 2 is peeled off from silicon chip surface using chemical etching method, white box part is single
Silicon nanowires local magnification region
Fig. 3 utilizes the silicon nanowires powder shown in Fig. 2 and bi powder and mg2The magnesium silicon substrate silicon nanowires compound thermal of si powder preparation
The section sem figure of electric material, brilliant white part is silicon nanowires
The transmission photo of Fig. 4 magnesium silicon substrate silicon nanowires composite thermoelectric material, the diffraction spot of in figure and white shown in arrow
The silicon nanowires in frame region is corresponding
The thermal conductivity of the magnesium silicon substrate silicon nanowires composite thermoelectric material of Fig. 5 different technical parameters preparation varies with temperature curve
Figure
Specific embodiment
Embodiment 1
Measure the agno that 20ml concentration is 0.035mol/l with graduated cylinder and dropper respectively3Solution and 20ml concentration are
The hf acid of 20wt.%, the two is mixed in beaker and is made into etching liquid 1.Twin polishing p-type monocrystalline by 10mm × 10mm
Silicon chip 2 is placed in etching liquid, etches 3h under normal temperature；Silicon chip after etching is to go at silver in 60wt.% red fuming nitric acid (RFNA) in 40ml concentration
Clean 5min with distilled water after reason, the silicon chip cleaning up 3 is placed in and fills 20ml ethanol solution 4 (water content ＜
Standby in beaker 0.03wt.%)；2g mixed powder, wherein mg is weighed in vacuum glove box2Si powder (purity > 99%,
Granularity≤850 μm) and bi powder (purity 99.99%, granularity≤75 μm) mole mixture ratio example be 0.99, mixed powder 5 is placed in
In solution 4；The beaker of solution 4 sonic oscillation 20min in supersonic wave cleaning machine 6 (model: ps-20) will be filled, then take out
Silicon chip, surplus solution 7 be placed in vacuum environment carry out on temperature control magnetic stirring apparatus 8 (model: 85-2) simultaneously magnetic agitation and
Vacuum drying, vacuum ＞ 0.09mpa, drying temperature is 35 DEG C, and the time is 120min；Powder after drying is placed in polytetrafluoro
In ethene ball grinder on planetary ball mill ball milling 4h, ratio of grinding media to material be 8:1, formed powder 9；Powder 9 is placed in a diameter of
In the graphite jig 10 of 20mm, in vacuum fapas stove, (vacuum ＞ 10pa) rises to 750 DEG C through 15min temperature, insulation
20min, in insulating process, pressure is 60mpa, after insulation terminates, closes electric current heating, release, sample along with the furnace cooling, obtains block
Bulk silicon nano line composite.
Embodiment 2
Measure the agno that 20ml concentration is 0.035mol/l with graduated cylinder and dropper respectively3Solution and 20ml concentration are
The hf acid of 20wt.%, the two is mixed in beaker and is made into etching liquid 1.Twin polishing p-type monocrystalline by 15mm × 20mm
Silicon chip 2 is placed in etching liquid, etches 4h under normal temperature；Silicon chip after etching is to go at silver in 60wt.% red fuming nitric acid (RFNA) in 40ml concentration
Clean 10min with distilled water after reason, the silicon chip cleaning up 3 is placed in and fills 20ml ethanol solution 4 (water content ＜
Standby in beaker 0.03wt.%)；2g mixed powder, wherein mg is weighed in vacuum glove box2Si powder (purity > 99%,
Granularity≤850 μm) and bi powder (purity 99.99%, granularity≤75 μm) mole mixture ratio example be 0.99, mixed powder 5 is placed in
In solution 4；The beaker of solution 4 sonic oscillation 25min in supersonic wave cleaning machine 6 (model: ps-20) will be filled, then take out
Silicon chip, surplus solution 7 be placed in vacuum environment carry out on temperature control magnetic stirring apparatus 8 (model: 85-2) simultaneously magnetic agitation and
Vacuum drying, vacuum ＞ 0.09mpa, drying temperature is 35 DEG C, and the time is 120min；Powder after drying is placed in polytetrafluoro
In ethene ball grinder on planetary ball mill ball milling 4h, ratio of grinding media to material be 8:1, formed powder 9；Powder 9 is placed in a diameter of
In the graphite jig 10 of 20mm, in vacuum fapas stove, (vacuum ＞ 10pa) rises to 750 DEG C through 15min temperature, insulation
20min, in insulating process, pressure is 60mpa, after insulation terminates, closes electric current heating, release, sample along with the furnace cooling, obtains block
Bulk silicon nano line composite.
Embodiment 3
Measure the agno that 20ml concentration is 0.035mol/l with graduated cylinder and dropper respectively3Solution and 20ml concentration are
The hf acid of 20wt.%, the two is mixed in beaker and is made into etching liquid 1.Twin polishing N-shaped monocrystalline by 10mm × 10mm
Silicon chip 2 is placed in etching liquid, etches 3h under normal temperature；Silicon chip after etching is to go at silver in 60wt.% red fuming nitric acid (RFNA) in 40ml concentration
Clean 5min with distilled water after reason, the silicon chip cleaning up 3 is placed in and fills 20ml ethanol solution 4 (water content ＜
Standby in beaker 0.03wt.%)；2g mixed powder, wherein mg is weighed in vacuum glove box2Si powder (purity > 99%,
Granularity≤850 μm) and bi powder (purity 99.99%, granularity≤75 μm) mole mixture ratio example be 0.99, mixed powder 5 is placed in
In solution 4；The beaker of solution 4 sonic oscillation 20min in supersonic wave cleaning machine 6 (model: ps-20) will be filled, then take out
Silicon chip, surplus solution 7 be placed in vacuum environment carry out on temperature control magnetic stirring apparatus 8 (model: 85-2) simultaneously magnetic agitation and
Vacuum drying, vacuum ＞ 0.09mpa, drying temperature is 35 DEG C, and the time is 120min；Powder after drying is placed in polytetrafluoro
In ethene ball grinder on planetary ball mill ball milling 4h, ratio of grinding media to material be 8:1, formed powder 9；Powder 9 is placed in a diameter of
In the graphite jig 10 of 20mm, in vacuum fapas stove, (vacuum ＞ 10pa) rises to 750 DEG C through 15min temperature, insulation
20min, in insulating process, pressure is 60mpa, after insulation terminates, closes electric current heating, release, sample along with the furnace cooling, obtains block
Bulk silicon nano line composite.
Contrast scheme
Without silicon nanowires in magnesium silica-base material, other operating process are identical with embodiment 1.
2g mixed powder, wherein mg is weighed in vacuum glove box2Si powder (purity > 99%, granularity≤850 μm) and bi
The mole mixture ratio example 0.99 of powder (purity 99.99%, granularity≤75 μm), forms mixed powder 5, mixed powder 5 is placed in poly-
In tetrafluoroethene ball grinder on planetary ball mill ball milling 4h, ratio of grinding media to material be 8:1, formed powder 9；Powder 9 is placed in diameter
In graphite jig 10 for 20mm, in vacuum fapas stove, (vacuum ＞ 10pa) rises to 750 DEG C through 15min temperature, insulation
20min, in insulating process, pressure is 60mpa, after insulation terminates, closes electric current heating, release, sample along with the furnace cooling, obtains block
Composite material.
Claims (1)
1. magnesium silicon substrate silicon nanowires composite thermoelectric material preparation method it is characterised in that be a kind of using silicon nanowires with
mg2Si thermoelectric material is combined and effectively reduces matrix thermal conductivity, is improved by adulterate sb, bi, la or ag and optimizes mg2Si sill
Thermoelectricity capability, synchronously realizes silicon nanowires stripping and mixing avoids silicon nanowires to be wound around in composite block material preparation and roll into a ball
Poly-, later stage electric field-assisted sintering process is prepared the magnesium silicon on silicon that silicon nanowire distribution is uniform and its is well combined with matrix
The method of nano wire composite thermoelectric material, the method is to utilize agno3Solution is etching liquid with the mixed liquor of hf acid, in monocrystalline silicon
On piece normal temperature etching 3h-4h prepare silicon nanowires, the silicon chip after etching go silver process cleaning after with purity > 99%, granularity≤
850μmmg2Si powder and the element that x is sb, bi, la or ag are placed in the ethanol solution of water content ＜ 0.03wt.% and surpass
Sound mixes, mixed solution drying and processing in the environment of vacuum ＞ 0.09mpa, and the powder after drying is carried out ball milling,
In order to avoid the pollution in mechanical milling process, using ball grinder and the zro of polytetrafluoroethylene (PTFE)2Abrading-ball, the powder after ball milling is placed in stone
In black mould, block nanometer is sintered into using fapas method and be combined hot material, specifically comprise the following steps that
1) measure agno respectively with graduated cylinder and dropper3Solution and hf acid, the two are mixed in beaker and are made into etching liquid (1),
Twin polishing monocrystalline silicon piece (2) is placed in etching liquid, under normal temperature, etches 3-4h；
2) silicon chip after etching goes silver to clean 5-10min with distilled water, by the silicon chip cleaning up (3) after processing in red fuming nitric acid (RFNA)
It is placed in standby in the beaker of ethanol solution (4), the water content ＜ 0.03wt.% of ethanol solution (4)；
3) weigh mg in vacuum glove box2Si powder, bi powder, by molal weight than the mg for x2Si powder and bi powder are mixed into
Powder (5) is placed in solution (4)；The scope than x for the molal weight is 0.96≤x≤0.99；
4) beaker of solution (4) sonic oscillation 20-25min in supersonic wave cleaning machine (6) will be filled, then take out silicon chip, remain
Remaining solution (7) is placed in vacuum environment and carries out magnetic agitation and vacuum drying, vacuum on temperature control magnetic stirring apparatus (8) simultaneously
＞ 0.09mpa, drying temperature is 35 DEG C, and the time is 120min;
5) powder after drying is placed in polytetrafluoroethylene (PTFE) ball grinder ball milling 4h on planetary ball mill, ratio of grinding media to material is 8:1,
Form powder (9)；
6) powder (9) is placed in graphite jig (10), through 15min temperature liter in the vacuum fapas stove of vacuum ＞ 10pa
To 750 DEG C, it is incubated 20min, in insulating process, pressure is 60mpa, after insulation terminates, close electric current heating, release, sample is with stove
Cooling.
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| CN101546805A (en) * | 2009-03-04 | 2009-09-30 | 中国科学院广州能源研究所 | Preparation method of high-quality-factor low-dimensional-oxide nanometer thermoelectric new material |
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| KR101409404B1 (en) * | 2012-10-09 | 2014-06-20 | 한양대학교 에리카산학협력단 | Manufacturing method for thermoelectric material and thermelectric material manufactured thereby |
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| CN101546805A (en) * | 2009-03-04 | 2009-09-30 | 中国科学院广州能源研究所 | Preparation method of high-quality-factor low-dimensional-oxide nanometer thermoelectric new material |
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| A simple phase transformation strategy for converting silicon nanowires into metal silicide nanowires:Magnesium silicide;Yongmin Kang;《Materials letters》;20130313;全文 * |
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