CN109384202A - One kind having room temperature inorganic electronic materials flexible and preparation method thereof - Google Patents
One kind having room temperature inorganic electronic materials flexible and preparation method thereof Download PDFInfo
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- CN109384202A CN109384202A CN201811452121.4A CN201811452121A CN109384202A CN 109384202 A CN109384202 A CN 109384202A CN 201811452121 A CN201811452121 A CN 201811452121A CN 109384202 A CN109384202 A CN 109384202A
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Abstract
The present invention develops a kind of prepare with room temperature Ag flexible for the first time2The method of Q (Q=Se, Te) base inorganic electronic materials, using Ag powder and Se or Te powder as raw material, Ag can high-volume be synthesized at room temperature by shaking up in the short time for it2Q (Q=Se, Te) single-phase compounds.Present invention firstly provides realize single-phase Ag using the simple means that shake up2The preparation of Q compound, and gained compound powder has good plasticity, can carry out simply cold pressing at room temperature and obtain the arbitrary shape bulk of high-compactness；Gained bulk also has good flexibility, big magneto-resistor and excellent thermoelectricity capability at room temperature, and a new thought can be provided for the preparation of high-performance flexible inorganic electronic materials.Preparation process of the present invention it is super it is simple, preparation time is ultrashort, can be for room temperature Ag flexible2High-volume preparing for Q inorganic electronic materials lays a good foundation with large-scale application.
Description
Technical field
The invention belongs to material science and technical fields, and in particular to one kind have room temperature inorganic electronic materials flexible and
Preparation method.
Background technique
Compared to conventional electronics, flexible electronic device have completely different mechanical property, including foldability, can
Draftability, flexible etc. cause great in numerous areas such as electronic device, photoelectric device, biological medicine and energy storages
It changes.Since the distortional stress of metal, alloy and organic material can achieve 5-100%, and hard and crisp inorganic partly lead
Body material is since crystal structure intrinsic property, distortional stress often only have 0.1-0.2%, rarely exceed 1%, so current is soft
Property electronic device is produced on organic/inorganic materials electronic device on flexibility/Drawability plastics or thin metal matrix plate.Therefore,
It seeks with room temperature inorganic semiconductor material flexible, for promoting the innovation of flexible electronic field to be of great significance.
Ag2Q (Q=Se, Te) compound is a kind of particularly important semiconductor material, has many peculiar electricity, light
And magnetic performance have potential application prospect.Currently, compound Ag2Se、Ag2The synthetic method of Te is concentrated mainly on hydro-thermal
Method, solvent-thermal method etc., these prepare Ag in the solution2Se、Ag2The method of Te, it is often necessary to complicated reaction process and stringent
Reaction condition.More regrettably, it needs to pollute environment using some toxic chemical reagent, time consumption and energy consumption.And it uses conventional
Long-time high-temperature melting method, high-temperature solid phase reaction method preparation, then to equipment requirement harshness, consume energy simultaneously, be easy to cause Se or
The missing of Te, it is difficult to be precisely controlled to point.In recent years, the Tang Xinfeng professor et al. of Wuhan University of Technology has been developed grinds at room temperature
Ag and Se/Te powder prepare Ag2The technology of Q (Q=Se, Te) compound, it is simple and fast.However grinding technics process mortar with grind
Friction between pestle inevitably brings localized hyperthermia's point, still could possibly be higher than Ag2Se and Ag2The transformation temperature of Te is (respectively
409K and 427K), the unordered Ag in the fast ion phase of temperature-fall period high temperature+Low-temperature phase intermediate gap position can be present in, so that
System carrier concentration is higher, deviates optimal carrier concentration, this is very unfavorable for the raising of thermoelectricity capability；In addition,
It is limited to the size of mortar itself, simple grinding technics is difficult disposably to prepare a large amount of samples (high-volume preparing), however, it is difficult to
Meet futurity industry demand.
Therefore, further seek a kind of Simple energy-saving, Ag that is environmentally protective, accurately controlling ingredient and micro-structure2Se、
Ag2Te and its high-volume technology of preparing, while realizing that its room temperature flexible application seems of crucial importance.
Summary of the invention
It is a kind of with room temperature inorganic electronic flexible it is a primary object of the present invention in view of the deficiencies of the prior art, provide
Material and preparation method thereof, the technique being related to it is super it is simple, preparation time is ultrashort, for room temperature Ag flexible2Q (Q=Se, Te)
High-volume preparing for inorganic electronic materials is had laid a good foundation with large-scale application.
To realize above scheme, the technical solution adopted by the present invention are as follows:
One kind having room temperature inorganic electronic materials flexible, it is Ag2Q (Q=Se or Te) based compound.
In above scheme, up to 20%, bending strain is reachable for compression strain at room temperature for the inorganic electronic materials
5%, in 60kOe, magneto-resistor is up to 200%, and dimensionless thermoelectric figure of merit ZT is up to 1.0 under room temperature.
In above scheme, the inorganic electronic materials are successively to be shaken up, suppressed using Ag powder, Q powder as raw material
Block Ag2Q (Q=Se or Te) material.
A kind of above-mentioned preparation method with room temperature inorganic electronic materials flexible, comprising the following steps:
1) using Ag powder, Q powder as raw material, two kinds of raw materials are shaken up at room temperature, i.e. synthesis Ag2Q (Q=Se or
Te) single-phase compounds powder；
2) by gained Ag2Q (Q=Se or Te) single-phase compounds powder is cold-pressed at room temperature, is obtained with room
Temperature inorganic electronic materials flexible.
In above scheme, the step that shakes up is shaken up or using manual using vortex mixer.
It is described to shake up time 18min or more in above scheme.
In above scheme, the cold pressing pressure is 300-800MPa, time 1-15min.
In above scheme, the Ag powder, Q powder molar ratio according to stoichiometric equation Ag2(1+x)Q, -0.01≤x≤0.2.
The principle of the present invention are as follows:
Present invention firstly provides the abilities for making full use of the extremely strong Dissociative Te in the surface Ag and Se steam, sharp at room temperature
It with simply technology is shaken up, adsorbs the saturated vapor of Te and Se by Ag surface dissociation, forms Ag2Te and Ag2Se compound；Together
When due to formation Ag2Te and Ag2Se product grain is very tiny (usually in nanoscale), Te and Se saturated vapor can be into one
This unsound product layer continuation of step infiltration reacts to form new Ag with the surface Ag2Te and Ag2Se compound, so circulation change
It is generation, finally that Ag is all depleted, entire reaction is completed, and be not necessarily to accessory external heat or mechanical force in reaction process, had
Effect avoids material system local temperature more high-leveled and difficult to be precisely controlled to point and the problems such as carrier concentration.
Compared with prior art, the invention has the benefit that
1) present invention firstly discloses one kind to have room temperature Ag flexible2Q (Q=Se, Te) base inorganic electronic materials, block
Material has good flexible, big magneto-resistor and excellent thermoelectricity capability at room temperature, and the preparation method being related to it is super it is simple, when
Between it is short, a new thought can be provided for the synthesis of room temperature flexible electronics.
2) for the present invention using Ag powder and Se or Te powder as raw material, Ag can be synthesized at room temperature by shaking up in the short time2Q (Q=Se,
Te) single-phase compounds powder, and accessory external heat or mechanical force are not necessarily in synthesis process between raw material, it can effectively avoid existing
It is easy to cause material system local temperature more high-leveled and difficult in heat treatment or mechanical force synthesis technology to be precisely controlled to point and carrier
The problem of concentration；And it is low to synthesis device requirement, it is suitble to high-volume produce.
3) using the Ag of preparation process of the present invention synthesis2Q (Q=Se, Te) single-phase compounds powder has good
Plasticity can carry out simply cold pressing at room temperature and obtain the arbitrary shape bulk of high-compactness, and applicability is wide.
Detailed description of the invention
Fig. 1 is the XRD spectrum of 1 step 2) products therefrom of embodiment.
Fig. 2 is the shape appearance figure of different shape block obtained by 1 step 3) of embodiment.
Fig. 3 is the scanning electron microscope (SEM) photograph of cutting particle obtained by 1 step 4) of embodiment.
Fig. 4 is 2 gained Ag of embodiment2The compression of Se block materials and bending stress-strain curve.
Fig. 5 is the magneto-resistor test result of 3 gained block materials phase transformation of embodiment before and after the processing.
Fig. 6 is 3 gained stoichiometric ratio Ag of embodiment2The block materials of Se (409K keeps the temperature 3min) sample after phase transformation is handled
The thermoelectricity capability test result of product.
Fig. 7 is 4 gained Ag of embodiment2The compression of Te block materials and bending stress-strain curve.
Fig. 8 is the magneto-resistor test result of 5 gained block materials phase transformation of embodiment before and after the processing.
Fig. 9 is 5 gained stoichiometric ratio Ag of embodiment2The block materials of Te (427K keeps the temperature 3min) sample after phase transformation is handled
The thermoelectricity capability test result of product.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
In following embodiment, Ag powder, Se, Te powder of use are commercial product, and granularity is 200 mesh, and purity is 5N.
Embodiment 1
One kind having room temperature inorganic electronic materials flexible, it is Ag2Q (Q=Se or Te) block materials, preparation method
Include the following steps:
1) using Ag powder and Q (Q=Se or Te) powder as raw material, Ag powder and Q powder are weighed by the molar ratio of 2:1 respectively,
Total 300g；
2) weighed raw material is placed in test tube, is subsequently placed in the quick vortex mixer of SK-1 type, setting mixes frequency and is
3000rpm, time 30min take out powder, carry out XRD analysis to it as shown in Figure 1, showing that gained powder is Ag2Se and
Ag2Te single-phase compounds；
3) by gained Ag2Se compound (or Ag2Te single-phase compounds) powder is fitted into different punching blocks, protects at 450MPa
Press 2min, can at room temperature cold compaction be up to for consistency 99.8% different shape block (Ag2Se block is shown in Fig. 2)；
4) by 20 × 0.2mm of Φ obtained by step 3)3Block Ag2Se carries out the cutting of different sized particles, and gained particle shines
Piece as shown in figure 3, smallest particles having a size of 0.13 × 0.13 × 0.2mm3, close to the cutting limit of cutting equipment, and particle side
Edge is sharp keen, and shape remains intact.
Above-described embodiment is analyzed, the present invention presents following prominent effect: a) shaking using the extremely simple room temperature short time
Even technology can prepare single-phase Ag2Se and Ag2Te compound；B) high cause can be prepared by simple room temperature cold press technique
The block materials of density, and the molding bulk of arbitrary shape can be obtained according to actual needs, show gained Ag2Se and Ag2Teization
Close the plasticity that powder has height；C) the bulk machining characteristics being prepared are superior, are easily obtainable small grain
Son, this is extremely advantageous for the production of microdevice.
Embodiment 2
One kind having room temperature inorganic electronic materials (Ag flexible2Se), preparation method includes the following steps:
1) using Ag powder and Se powder as raw material, Ag powder and Se powder are weighed by the molar ratio of 2:1, total 15g；
2) weighed raw material is placed in Φ 50mm test tube, then test tube open end is sealed, rear vertical direction fluctuates
Test tube, frequency are about 60 times/min, and shaking up the time is 24min, take out powder, obtain Ag2Se powder；
3) by gained Ag2Se powder is fitted into 20 punching block of Φ, the pressure maintaining 2min at 500MPa, can cold compaction at room temperature
Standby consistency is up to 99.7% block materials, and block thickness design is at 3mm and 2mm.
Block materials obtained by the present embodiment are cut into 3 × 3 × 6mm3With 2 × 2 × 15mm3Specification, after stringent polishing point
Compression and crooked experiment are not carried out, and gained load-deformation curve is as shown in Figure 4 at room temperature.
From fig. 4, it can be seen that gained Ag2There is one section of plasticity and become in the compression of Se bulk and bending stress-strain curve
Shape region, material is just broken later, and maximum compression and bending strain are respectively 15.2% and 4%, it can be seen that, gained Ag2Se
Bulk has certain flexibility at room temperature, is greatly different from the brittleness at room temperature fracture of general inorganic material.
Embodiment 3
One kind having room temperature inorganic electronic materials (Ag flexible2Se), preparation method includes the following steps:
1) using Ag powder and Se powder as raw material, stoichiometrically Ag2(1+x)Se (x=0,0.002,0.006 or 0.01) is carried out
It weighs, respectively 10g；
2) weighed raw material is placed in test tube, is subsequently placed in the quick vortex mixer of SK-1 type, setting mixes frequency and is
2000rpm, time 18min take out powder, obtain Ag2Se powder；
3) by gained Ag2Se powder is respectively charged into 20 punching block of Φ, the pressure maintaining 2min at 480MPa, can be cold at room temperature
The block materials that standby consistency is up to 99.8% are suppressed, block thickness design is at 2mm.
By disc-shaped Ag obtained by the present embodiment2Se is divided into two, and wherein half will be warming up to 409K, and keep the temperature 3min, into
Row phase transformation processing；By the semicircle sheet Ag after before phase change2Se is cut into 2 × 1 × 8mm3Strip carries out the test of magneto-resistor, as a result
As shown in Figure 5.
Choose stoichiometric ratio Ag2The block materials of Se (409K keeps the temperature 3min) sample after phase transformation is handled carries out pyroelectricity
It can test, as a result as shown in Figure 6.
As shown in Figure 5, each sample is shown as linearly at highfield, and shows unsaturated feature.Work as x=0.01
When, for phase transformation treated sample under the magnetic field 60kOe, magnetoresistive ratio is up to 70%.It will be appreciated from fig. 6 that as x=0, through phase
Becoming treated sample in 300K, ZT is up to 0.91 (significantly larger than existing research level, such as patent CN105256161),
In 390K, ZT is up to 1.3, can be with commercialized Bi2Te3Basal cell's warm electric material compares favourably.
The above results show that gained block materials of the invention have excellent thermo-electrically-magnetic property, and test shows gained
Block materials have good room temperature flexible.
Embodiment 4
One kind having room temperature inorganic electronic materials (Ag flexible2Te), preparation method includes the following steps:
1) using Ag powder and Te powder as raw material, Ag powder and Te powder are weighed by the molar ratio of 2:1, total 15g；
2) weighed raw material is placed in test tube, is subsequently placed in the quick vortex mixer of SK-1 type, setting mixes frequency and is
1500rpm, time 20min take out powder, obtain Ag2Te powder；
3) by gained Ag2Te powder is fitted into 20 punching block of Φ, the pressure maintaining 2min at 500MPa, can cold compaction at room temperature
Standby consistency is up to 99.7% block materials, and block thickness design is at 3mm and 2mm.
Block materials obtained by the present embodiment are cut into 3 × 3 × 6mm3And 2 × 2 × 15mm3Specification, after stringent polishing point
Compression and crooked experiment are not carried out, and load-deformation curve is as shown in Figure 7 at room temperature.
From figure 7 it can be seen that Ag2There is one section of plastically deforming area in the compression of Te bulk and bending stress-strain curve
Domain, material is just broken later, and maximum compression and bending strain are respectively 14% and 3%, it can be seen that, Ag2Te bulk is in room temperature
There is down certain flexibility, be greatly different from the brittleness at room temperature fracture of general inorganic material.
Embodiment 5
One kind having room temperature inorganic electronic materials (Ag flexible2Te), preparation method includes the following steps:
1) using Ag powder and Te powder as raw material, stoichiometrically Ag2(1+x)Te (x=0,0.002,0.006,0.025,0.1
Or it 0.2) is weighed, respectively 10g；
2) weighed raw material is placed in test tube, is subsequently placed in the quick vortex mixer of SK-1 type, setting mixes frequency and is
2000rpm, time 18min take out powder；Ag is obtained respectively2Te powder；
3) by gained Ag2Te powder is respectively charged into 20 punching block of Φ, the pressure maintaining 2min at 480MPa, can be cold at room temperature
The block materials that standby consistency is up to 99.8% are suppressed, block thickness design is at 2mm；
By disc-shaped Ag obtained by the present embodiment2Te is divided into two, and wherein half will be warming up to 427K, and keep the temperature 3min, into
Row phase transformation processing；By the semicircle sheet Ag after before phase change2Te is cut into 2 × 1 × 8mm3Strip carries out the test of magneto-resistor, as a result
As shown in Figure 8.
Selection stoichiometric ratio is Ag2The bulk material of Te (427K keeps the temperature 3min) sample after phase transformation is handled carries out thermoelectricity
Performance test, as a result as shown in Figure 9.
As shown in Figure 8, each sample is shown as linearly at highfield, and shows unsaturated feature.Before phase transformation processing,
For x=0 and x=0.2 sample under the magnetic field 60kOe, magnetoresistive ratio is up to 38% and 44% respectively.After phase transformation is handled, x=
For 0 and x=0.2 sample under the magnetic field 60kOe, magnetoresistive ratio is up to 113% and 153%.
As shown in Figure 9, as x=0, through phase transformation, treated that sample is very superior near room temperature thermoelectricity capability,
When 300K, ZT is up to 0.54, and in 400K, ZT is up to 0.84.
The above results show that gained block materials of the invention have excellent thermo-electrically-magnetic property, and test shows gained
Block materials have good room temperature flexible.
The above is only a preferred embodiment of the present invention, it is noted that come for those of ordinary skill in the art
It says, without departing from the concept of the premise of the invention, several modifications and variations can also be made, these belong to of the invention
Protection scope.
Claims (7)
1. one kind has room temperature inorganic electronic materials flexible, it is Ag2Q based compound, wherein Q=Se or Te.
2. inorganic electronic materials according to claim 1, which is characterized in that the inorganic electronic materials are with Ag powder, Q powder
For raw material, the block Ag for successively being shaken up, being suppressed2Q material, wherein Q=Se or Te.
3. the preparation method as claimed in claim 1 or 2 with room temperature inorganic electronic materials flexible, which is characterized in that including with
Lower step:
1) using Ag powder, Q powder as raw material, Q=Se or Te at room temperature shake up two kinds of raw materials, synthesize Ag2Q single-phaseization
Close powder；
2) by gained Ag2Q single-phase compounds powder is cold-pressed at room temperature, is obtained with room temperature inorganic electronic flexible
Material.
4. preparation method according to claim 3, which is characterized in that the step that shakes up is shaken up or using manual using mixed
Even device.
5. preparation method according to claim 3, which is characterized in that described to shake up the time as 18min or more.
6. preparation method according to claim 3, which is characterized in that the cold pressing pressure is 300-800MPa, and the time is
1-15min。
7. preparation method according to claim 3, which is characterized in that the Ag powder, Q powder are according to Ag2(1+x)The chemistry meter of Q
Amount ratio is weighed, wherein Q=Se or Te, -0.01≤x≤0.2.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112458420A (en) * | 2020-11-30 | 2021-03-09 | 北京信息科技大学 | Silver telluride-silver sulfide film with nanorod array and preparation method thereof |
| CN113353897A (en) * | 2020-03-04 | 2021-09-07 | 武汉理工大学 | Superplastic Ag2Preparation method of Se nano ultrafine crystal thermoelectric material |
-
2018
- 2018-11-30 CN CN201811452121.4A patent/CN109384202B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| JIE GAO ET AL.: "A novel glass-fiber-aided cold-press method for fabrication of n-type Ag2Te nanowires thermoelectric film on fiexible copy-paper substrate", 《J.MATER.CHEM.A》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113353897A (en) * | 2020-03-04 | 2021-09-07 | 武汉理工大学 | Superplastic Ag2Preparation method of Se nano ultrafine crystal thermoelectric material |
| CN113353897B (en) * | 2020-03-04 | 2024-03-26 | 武汉理工大学 | Superplastic Ag 2 Preparation method of Se nanometer superfine crystal thermoelectric material |
| CN112458420A (en) * | 2020-11-30 | 2021-03-09 | 北京信息科技大学 | Silver telluride-silver sulfide film with nanorod array and preparation method thereof |
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