CN107604208A - Device is got rid of in a kind of method for preparing p-type filled skutterudite compound and melt rotation - Google Patents
Device is got rid of in a kind of method for preparing p-type filled skutterudite compound and melt rotation Download PDFInfo
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- CN107604208A CN107604208A CN201710875549.9A CN201710875549A CN107604208A CN 107604208 A CN107604208 A CN 107604208A CN 201710875549 A CN201710875549 A CN 201710875549A CN 107604208 A CN107604208 A CN 107604208A
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Abstract
The invention belongs to skutterudite compound preparing technical field, discloses a kind of method for preparing p-type filled skutterudite compound and device is got rid of in melt rotation, including：The sample weighed using stoichiometric proportion is placed in the graphite-pipe of bottom, using high-frequency electromagnetic induction mode of heating, it is liquid that sample melted is made in very short time as initiation material；Apply whiff pressure Ar gases above melt, melt can quickly be ejected into the copper roller surface of rotation at a high speed from aperture, while quick chilling and form continuous band-shaped amorphous or nanocrystalline material；Gained is got rid of into carry sample grinding afterwards, plasma discharging spark sintering obtains the good block materials of compactness.The preparation speed of the present invention is fast, can effectively improve sample preparation efficiency, suppress the volatilization of effumability element；Rotation is got rid of equipment and is placed in the glove box that Ar atmosphere is enclosed, and can effectively prevent the generation of oxide dephasign；Gained sample crystallite dimension is tiny, composition is uniform, can obviously reduce the lattice thermal conductivity of material.
Description
Technical field
The invention belongs to skutterudite compound preparing technical field, more particularly to one kind to prepare p-type filled skutterudite
Device is got rid of in method and the melt rotation of compound.
Background technology
Pure phase p-type filled skutterudite compound prepared by conventional solid reaction method not only requires a great deal of time
(general 8 days or so), and the sample thermal conductivity that this method is prepared is of a relatively high because the sample size for preparing of this method compared with
Greatly, crystal grain distribution is uneven, grain boundary density is smaller, and the scattering process to phonon is weaker.We can by using independent research
The melt rotation being placed in glove box get rid of device successfully synthesized within the time less than 3h composition uniformly, crystal grain refinement, crystal boundary it is close
The higher single-phase p-type filled skutterudite compound of degree, enhance phon scattering effect.This method not only substantially reduces preparation
Cycle (being foreshortened to from 8 days 3 hours), cost is reduced, and sample thermal conductivity is also greatly reduced.
In summary, the problem of prior art is present be：Pure phase p-type filled skutterudite prepared by conventional solid reaction method
Compound not only requires a great deal of time, and the sample thermal conductivity that this method is prepared is of a relatively high.We are by making
Device is got rid of with the melt being placed in the glove box rotation of independent research and quickly prepares single-phase p-type filled skutterudite compound, no
Only substantially reduce manufacturing cycle, reduce cost, and sample thermal conductivity is also greatly reduced.
The content of the invention
The problem of existing for prior art, the invention provides a kind of side for preparing p-type filled skutterudite compound
Device is got rid of in method and melt rotation.
The present invention is achieved in that a kind of method for preparing p-type filled skutterudite compound, and the preparation p-type is filled out
The method for filling formula skutterudite compound comprises the following steps：
Step 1, the sample weighed using stoichiometric proportion are placed in the graphite-pipe of bottom, using high-frequency electrical as initiation material
The mode of magnetic induction heating (800 degrees Celsius~1200 degrees Celsius), it is liquid that sample melted is made in very short time；
Step 2, applies the high-purity Ar gas of whiff pressure above melt, and melt quickly can be ejected into from aperture
The copper roller surface of rotation at a high speed, at the same quick chilling and form continuous band-shaped amorphous or nanocrystalline material；Gained is got rid of into band sample afterwards
Product grinding, plasma discharging spark sintering obtain the good block materials of compactness.
Further, the graphite-pipe that aperture is 0.1~1mm is left in bottom in the step 1.
Further, the high-purity Ar gas of 0.5-2Mpa whiff pressures is applied in the step 2 above melt.
Another object of the present invention is to provide a kind of melt rotation for preparing p-type filled skutterudite compound and using
Device is got rid of, device is got rid of in the melt rotation to be included：Graphite-pipe, high-frequency electromagnetic induction heater, copper roller, motor.
Advantages of the present invention and good effect are：Device is got rid of in melt rotation realizes the supper-fast preparation of material, reduces into
This, preparation time foreshortened to 3 hours from 8 days.The preparation speed of the present invention is fast, can effectively improve sample preparation efficiency, suppress easy
The volatilization of volatile element；Rotation is got rid of equipment and is placed in the glove box that Ar atmosphere is enclosed, and can effectively prevent the generation of oxide dephasign；Institute
Sample crystallite dimension is tiny, composition is uniform, can obviously reduce the lattice thermal conductivity of material.
Brief description of the drawings
Fig. 1 is the method flow diagram of preparation p-type filled skutterudite compound provided in an embodiment of the present invention.
Fig. 2 is that apparatus structure schematic diagram is got rid of in melt rotation provided in an embodiment of the present invention；
In figure：1st, graphite-pipe；2nd, high-frequency electromagnetic induction heater；3rd, motor；4th, copper roller.
Fig. 3 is cobalt ore compound field emission scanning electron microscope comparing result schematic diagram provided in an embodiment of the present invention；
(b) it is the p-type filled type side cobalt provided in an embodiment of the present invention with obtained figure (a) same composition of conventional solid-state method
Mineralising compound field emission scanning electron microscope comparing result schematic diagram.
Fig. 4 is the p-type filled skutterudite of same composition provided in an embodiment of the present invention made from conventional solid-state method
Compound lattice thermal conductivity comparing result schematic diagram.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The application principle of the present invention is explained in detail below in conjunction with the accompanying drawings.
As shown in figure 1, the method provided in an embodiment of the present invention for preparing p-type filled skutterudite compound includes following step
Suddenly：
S101：The sample weighed using stoichiometric proportion is placed in bottom and leaves the stone that aperture is 0.1-1mm as initiation material
Mo Guanzhong, by the way of high-frequency electromagnetic induction heating, it is liquid that sample melted is made in very short time；
S102：Apply the high-purity Ar gas of 0.5-2Mpa whiff pressures above melt, melt can be quickly from aperture
Be ejected into the copper roller surface of rotation at a high speed, at the same quick chilling and form continuous band-shaped amorphous or nanocrystalline material；Afterwards by gained
Get rid of carry sample grinding, plasma discharging spark sintering obtains the good block materials of compactness.
As shown in Fig. 2 melt rotation provided in an embodiment of the present invention is got rid of device and included：Graphite-pipe 1, high-frequency electromagnetic induction heating
Device 2, motor 3, copper roller 4.
The outside of graphite-pipe 1 is cased with high-frequency electromagnetic induction heater 2, and motor 3 connects copper roller 4.
The method provided in an embodiment of the present invention for preparing p-type filled skutterudite compound need or so 3 hours (including
Weigh)；The uniform sample of crystal grain refinement, composition (shown in such as Fig. 3 (b)) is obtained, and sample lattice thermal conductivity is significantly lower than tradition
The sample lattice thermal conductivity (as shown in Figure 4) that method measures, conducting material thermoelectricity performance is significantly improved.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (6)
- A kind of 1. method for preparing p-type filled skutterudite compound, it is characterised in that the preparation p-type filled skutterudite The method of compound comprises the following steps：Step 1, the sample weighed using stoichiometric proportion are placed in graphite-pipe, heated using high-frequency electromagnetic induction as initiation material Mode, it is liquid that sample melted is made in very short time；Step 2, applies the high-purity Ar gas of whiff pressure above melt, and melt quickly can be ejected at a high speed from aperture The copper roller surface of rotation, at the same quick chilling and form continuous band-shaped amorphous or nanocrystalline material；Gained is got rid of into carry sample afterwards to grind Mill, plasma discharging spark sintering obtain the good block materials of compactness.
- 2. the method for p-type filled skutterudite compound is prepared as claimed in claim 1, it is characterised in that the step 1 Middle raw material is Fe, Co, Sb, R, and the R in raw material Fe, Co, Sb, R is periodic table of elements middle rare earth metal, alkali metal and alkaline earth gold The combination of a kind of element or multiple element of category.
- 3. the method for p-type filled skutterudite compound is prepared as claimed in claim 1, it is characterised in that the step 1 Middle raw material matches by mol is：R:(Fe+Co):Sb=(0~1):4:(11~13).
- 4. the method for p-type filled skutterudite compound is prepared as claimed in claim 1, it is characterised in that the step 1 Leave the graphite-pipe that aperture is 0.1~1mm in middle bottom.
- 5. the method for p-type filled skutterudite compound is prepared as claimed in claim 1, it is characterised in that the step 2 In above melt apply 0.5-2Mpa whiff pressures high-purity Ar gas.
- 6. device is got rid of in the melt rotation that a kind of method for preparing p-type filled skutterudite compound as claimed in claim 1 uses, its It is characterised by, device is got rid of in the melt rotation to be included：Graphite-pipe, high-frequency electromagnetic induction heater, copper roller, motor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710875549.9A CN107604208A (en) | 2017-09-25 | 2017-09-25 | Device is got rid of in a kind of method for preparing p-type filled skutterudite compound and melt rotation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710875549.9A CN107604208A (en) | 2017-09-25 | 2017-09-25 | Device is got rid of in a kind of method for preparing p-type filled skutterudite compound and melt rotation |
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| CN107604208A true CN107604208A (en) | 2018-01-19 |
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| CN201710875549.9A Pending CN107604208A (en) | 2017-09-25 | 2017-09-25 | Device is got rid of in a kind of method for preparing p-type filled skutterudite compound and melt rotation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114082968A (en) * | 2021-10-26 | 2022-02-25 | 广州大学 | Method for large-scale preparation of filled skutterudite material by spray rotary quenching |
| CN117715497A (en) * | 2024-02-06 | 2024-03-15 | 乌镇实验室 | Antioxidant skutterudite-based thermoelectric composite material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101693962A (en) * | 2009-10-19 | 2010-04-14 | 武汉理工大学 | Method for preparing p-type filling type skutterudite compound thermoelectric material |
-
2017
- 2017-09-25 CN CN201710875549.9A patent/CN107604208A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101693962A (en) * | 2009-10-19 | 2010-04-14 | 武汉理工大学 | Method for preparing p-type filling type skutterudite compound thermoelectric material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114082968A (en) * | 2021-10-26 | 2022-02-25 | 广州大学 | Method for large-scale preparation of filled skutterudite material by spray rotary quenching |
| CN114082968B (en) * | 2021-10-26 | 2023-08-29 | 广州大学 | Method for preparing filled skutterudite material in large scale by spray spin quenching |
| CN117715497A (en) * | 2024-02-06 | 2024-03-15 | 乌镇实验室 | Antioxidant skutterudite-based thermoelectric composite material and preparation method thereof |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180119 |
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| RJ01 | Rejection of invention patent application after publication |