CN105174743B - FeS2Thin-film material and preparation method thereof - Google Patents
FeS2Thin-film material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of FeS2Thin-film material and preparation method thereof, including the 1) dielectric layer on silicon sheet or quartzy thin slice；2) continue to deposit iron thin film on the dielectric layer again, obtain plating iron predecessor；3) the plating iron predecessor is positioned over to the downstream of heating furnace, sulphur is positioned over to the upstream of heating furnace, inert gas is passed through to heating furnace, sulphur is heated to 130~180 DEG C, sulphur is evaporated to sulfur gas, and as inert gas enters the downstream of heating furnace；4) heating furnace is risen into reaction temperature with 5~15 DEG C/min of programming rate, keeps temperature to be reacted, be FeS by iron thin film vulcanization2, that is, obtain the FeS2Thin-film material.The feasibility of the preparation method is high, preparation method is simple, production cost is low, is easy to industrialized mass production, while the FeS prepared2Thin-film material can be widely applied in various electronics, energy field.
Description
Technical field
The present invention relates to nano film material technical field, and in particular to a kind of FeS2Thin-film material and preparation method thereof.
Background technology
FeS2, be otherwise known as fool's gold or chalcopyrite, is a kind of extremely abundant mineral products, usually in quartz vein, sedimentary rock
It is found with coal seam, itself is also a semiconductor to have a great attraction.From the seventies in last century, just there is substantial amounts of research
Concentrate FeS2Application in terms of solar cell.Its band gap is smaller, between 0.8~0.95eV, and absorptivity
Very big (α=6 × 105cm-1, h υ ＞ 1.3eV), become a kind of very promising solar energy transition material.
And the highest electronic carrier mobility reported at present is about 360cm2V-1s-1, while minority carrier diffusion length
Spend for 0.1~1 μm.But current FeS2Solar cell highest energy conversion ratio be only 3%.Researcher is having found to lead
It is that its material has a substantial amounts of surface defect to want problem, at the same in material crystalline substance as purity it is inadequate.At the same time, although research is numerous,
But there was only very a small number of research by FeS2Using in the application of diode.Also, the performance of these diodes is relatively
Difference, without switching characteristic.
The content of the invention
In view of this, it is an object of the invention to propose a kind of FeS2Thin-film material and preparation method thereof, to improve material
Crystalline substance as purity.
Based on above-mentioned purpose, FeS provided by the invention2The preparation method of thin-film material comprises the following steps：
1) dielectric layer on silicon sheet or quartzy thin slice；
2) continue to deposit iron thin film on the dielectric layer again, obtain plating iron predecessor；
3) the plating iron predecessor is positioned over to the downstream of heating furnace, sulphur is positioned over to the upstream of heating furnace, to heating
Stove is passed through inert gas, sulphur is heated to 130~180 DEG C, sulphur is evaporated to sulfur gas, and adds as inert gas enters
The downstream of hot stove；
4) heating furnace is risen into reaction temperature with 5~25 DEG C/min of programming rate, keeps temperature to be reacted, by iron
Film vulcanization is FeS2, that is, obtain the FeS2Thin-film material.
In some embodiments of the invention, in the step 1), using Low Pressure Chemical Vapor Deposition, sputtering method and
At least one of plasma deposition processes method is by dielectric layer deposition on silicon sheet or quartzy thin slice.
In some embodiments of the invention, the thickness of the dielectric layer is
In some embodiments of the invention, the dielectric material of the dielectric layer is selected from SiO2, Al2O3, ZrO2And HfO2
At least one of.
In some embodiments of the invention, in the step 2), using in electron beam evaporation deposition method and sputtering method
At least one method continue on the dielectric layer deposit iron thin film.
In some embodiments of the invention, the thickness of the iron thin film is
In some embodiments of the invention, the inert gas is selected from argon gas, nitrogen.
In some embodiments of the invention, the flow velocity of the inert gas is 20~500sccm.
In some embodiments of the invention, in the step 4), the reaction temperature of heating furnace is 200~800 DEG C,
When reaction time is 2~8 small.
The present invention also provides a kind of FeS2Thin-film material, the FeS2Thin-film material is according to above-mentioned FeS2The system of thin-film material
Preparation Method is made.
From the above it can be seen that FeS provided by the invention2Thin-film material is using first depositing iron thin film, then by its sulphur
Turn to FeS2The method of film is prepared, and the preparation method is simple, and cost is low, and obtained FeS2The brilliant picture of thin-film material
Purity is high, can adjust and adapt to a variety of environment and condition, has to scientific research and other large-scale productions aspects potential
Application.The feasibility of the preparation method is high, preparation method is simple, production cost is low, is easy to industrialized mass production, makes at the same time
Standby FeS out2Thin-film material can be widely applied in various electronics, energy field.
Brief description of the drawings
Fig. 1 is the consersion unit structure chart of the embodiment of the present invention；
Fig. 2 is the FeS of the embodiment of the present invention2The XRD spectrum of thin-film material；
Fig. 3 is the FeS of the embodiment of the present invention2The Raman collection of illustrative plates of thin-film material.
Embodiment
For the object, technical solutions and advantages of the present invention are more clearly understood, below in conjunction with specific embodiment, and reference
Attached drawing, the present invention is described in more detail.
Embodiment 1
First, use Low Pressure Chemical Vapor Deposition on 4 inches of silicon sheet deposit thickness forSiO2As
Dielectric layer, then using electron beam evaporation deposition method in obtained SiO2Continuing deposit thickness on/Si substrates isIron
Film, as plating iron predecessor.
Then, the plating iron predecessor is positioned over to the downstream of tube furnace, the upstream of tube furnace is placed with aluminium oxide ceramics earthenware
Crucible, and 1.5 grams of sulphur powder are added, boiler tube external application silica gel heating band parcel, and connect temperature control device.Afterwards, lead to tube furnace
Enter argon gas, speed 200sccm, as shown in Figure 1.Tube furnace, when tube furnace is raised to 200 DEG C, is opened with 10 DEG C/min of heatings
Heating tape, makes the sulphur powder in crucible be warming up to 160 DEG C, sulphur powder is evaporated to sulfur gas, and is managed as argon gas enters
The downstream of formula stove.Sulphur required temperature and the heating-up temperature of tube furnace are different, thus need the upstream of tube furnace it is external plus
The torrid zone, for heating sulphur.
After 50 minutes, tube furnace rises to 500 DEG C with 12 DEG C/min of programming rate, keep temperature carry out reaction 3 it is small when,
It is FeS by iron thin film vulcanization2, that is, obtain the FeS2Thin-film material.After reaction, close and remove heating tape, wait tube furnace
Room temperature is naturally cooling to, tube furnace is opened and takes out the FeS after reaction2Thin-film material.
Embodiment 2
First, use sputtering method on 4.5 inches of silicon sheet deposit thickness forSiO2As dielectric layer, so
Afterwards using sputtering method in obtained SiO2Continuing deposit thickness on/Si substrates isIron thin film, as plating iron forerunner
Thing.
Then, the plating iron predecessor is positioned over to the downstream of tube furnace, the upstream of tube furnace is placed with aluminium oxide ceramics earthenware
Crucible, and 1.8 grams of sulphur powder are added, boiler tube external application silica gel heating band parcel, and connect temperature control device.Afterwards, lead to tube furnace
Enter argon gas, speed 150sccm, as shown in Figure 1.Tube furnace, when tube furnace is raised to 180 DEG C, is opened with 8 DEG C/min of heatings
Heating tape, makes the sulphur powder in crucible be warming up to 150 DEG C, sulphur powder is evaporated to sulfur gas, and is managed as argon gas enters
The downstream of formula stove.
After sixty minutes, tube furnace rises to 600 DEG C with 15 DEG C/min of programming rate, keep temperature carry out reaction 4 it is small when,
It is FeS by iron thin film vulcanization2, that is, obtain the FeS2Thin-film material.After reaction, close and remove heating tape, wait tube furnace
Room temperature is naturally cooling to, tube furnace is opened and takes out the FeS after reaction2Thin-film material.
Embodiment 3
First, use Low Pressure Chemical Vapor Deposition on 4 inches of quartzy thin slice deposit thickness forZrO2Make
For dielectric layer, then using electron beam evaporation deposition method in obtained ZrO2/SiO2Continuing deposit thickness on substrate is
Iron thin film, as plating iron predecessor.
Then, the plating iron predecessor is positioned over to the downstream of tube furnace, the upstream of tube furnace is placed with aluminium oxide ceramics earthenware
Crucible, and 1.7 grams of sulphur powder are added, boiler tube external application silica gel heating band parcel, and connect temperature control device.Afterwards, lead to tube furnace
Enter nitrogen, speed 250sccm, as shown in Figure 1.Tube furnace, when tube furnace is raised to 200 DEG C, is opened with 11 DEG C/min of heatings
Heating tape, makes the sulphur powder in crucible be warming up to 165 DEG C, sulphur powder is evaporated to sulfur gas, and is managed as nitrogen enters
The downstream of formula stove.
After 45 minutes, tube furnace rises to 480 DEG C with 12 DEG C/min of programming rate, keep temperature carry out reaction 6 it is small when,
It is FeS by iron thin film vulcanization2, that is, obtain the FeS2Thin-film material.After reaction, close and remove heating tape, wait tube furnace
Room temperature is naturally cooling to, tube furnace is opened and takes out the FeS after reaction2Thin-film material.
Embodiment 4
First, use plasma deposition processes on 3.2 inches of quartzy thin slice deposit thickness forAl2O3As
Dielectric layer, then using electron beam evaporation deposition method in obtained Al2O3/SiO2Continuing deposit thickness on substrate is's
Iron thin film, as plating iron predecessor.
Then, the plating iron predecessor is positioned over to the downstream of tube furnace, the upstream of tube furnace is placed with aluminium oxide ceramics earthenware
Crucible, and 1.4 grams of sulphur powder are added, boiler tube external application silica gel heating band parcel, and connect temperature control device.Afterwards, lead to tube furnace
Enter argon gas, speed 100sccm, as shown in Figure 1.Tube furnace, when tube furnace is raised to 190 DEG C, is opened with 6 DEG C/min of heatings
Heating tape, makes the sulphur powder in crucible be warming up to 170 DEG C, sulphur powder is evaporated to sulfur gas, and is managed as argon gas enters
The downstream of formula stove.
After 45 minutes, tube furnace rises to 800 DEG C with 10 DEG C/min of programming rate, keep temperature carry out reaction 5 it is small when,
It is FeS by iron thin film vulcanization2, that is, obtain the FeS2Thin-film material.After reaction, close and remove heating tape, wait tube furnace
Room temperature is naturally cooling to, tube furnace is opened and takes out the FeS after reaction2Thin-film material.
Embodiment 5
First, use Low Pressure Chemical Vapor Deposition on 5.5 inches of quartzy thin slice deposit thickness forHfO2
As dielectric layer, then using sputtering method in obtained HfO2/SiO2Continuing deposit thickness on substrate isIron it is thin
Film, as plating iron predecessor.
Then, the plating iron predecessor is positioned over to the downstream of tube furnace, the upstream of tube furnace is placed with aluminium oxide ceramics earthenware
Crucible, and 2.2 grams of sulphur powder are added, boiler tube external application silica gel heating band parcel, and connect temperature control device.Afterwards, lead to tube furnace
Enter argon gas, speed 600sccm, as shown in Figure 1.Tube furnace, when tube furnace is raised to 190 DEG C, is opened with 15 DEG C/min of heatings
Heating tape, makes the sulphur powder in crucible be warming up to 160 DEG C, sulphur powder is evaporated to sulfur gas, and is managed as argon gas enters
The downstream of formula stove.
After 45 minutes, tube furnace rises to 200 DEG C with 10 DEG C/min of programming rate, keeps temperature to carry out reaction 7.5 small
When, it is FeS by iron thin film vulcanization2, that is, obtain the FeS2Thin-film material.After reaction, close and remove heating tape, wait pipe
Formula stove is naturally cooling to room temperature, opens tube furnace and takes out the FeS after reaction2Thin-film material.
Embodiment 6
First, use plasma deposition processes on 4 inches of silicon sheet deposit thickness forZrO2As dielectric
Layer, then using electron beam evaporation deposition method in obtained ZrO2Continuing deposit thickness on/Si substrates isIron it is thin
Film, as plating iron predecessor.
Then, the plating iron predecessor is positioned over to the downstream of tube furnace, the upstream of tube furnace is placed with aluminium oxide ceramics earthenware
Crucible, and 1.7 grams of sulphur powder are added, boiler tube external application silica gel heating band parcel, and connect temperature control device.Afterwards, lead to tube furnace
Enter nitrogen, speed 450sccm, as shown in Figure 1.Tube furnace, when tube furnace is raised to 198 DEG C, is opened with 8 DEG C/min of heatings
Heating tape, makes the sulphur powder in crucible be warming up to 165 DEG C, sulphur powder is evaporated to sulfur gas, and is managed as nitrogen enters
The downstream of formula stove.
After sixty minutes, tube furnace rises to 400 DEG C with 12 DEG C/min of programming rate, keeps temperature to carry out reaction 4.5 small
When, it is FeS by iron thin film vulcanization2, that is, obtain the FeS2Thin-film material.After reaction, close and remove heating tape, wait pipe
Formula stove is naturally cooling to room temperature, opens tube furnace and takes out the FeS after reaction2Thin-film material.
Embodiment 7
First, use sputtering method on 4 inches of silicon sheet deposit thickness forHfO2As dielectric layer, then
Using electron beam evaporation deposition method in obtained HfO2Continuing deposit thickness on/Si substrates isIron thin film, as plating
Iron predecessor.
Then, the plating iron predecessor is positioned over to the downstream of tube furnace, the upstream of tube furnace is placed with aluminium oxide ceramics earthenware
Crucible, and 1.3 grams of sulphur powder are added, boiler tube external application silica gel heating band parcel, and connect temperature control device.Afterwards, lead to tube furnace
Enter nitrogen, speed 240sccm, as shown in Figure 1.Tube furnace, when tube furnace is raised to 220 DEG C, is opened with 23 DEG C/min of heatings
Heating tape, makes the sulphur powder in crucible be warming up to 175 DEG C, sulphur powder is evaporated to sulfur gas, and is managed as nitrogen enters
The downstream of formula stove.
After 30 minutes, tube furnace rises to 280 DEG C with 15 DEG C/min of programming rate, keeps temperature to carry out reaction 6.5 small
When, it is FeS by iron thin film vulcanization2, that is, obtain the FeS2Thin-film material.After reaction, close and remove heating tape, wait pipe
Formula stove is naturally cooling to room temperature, opens tube furnace and takes out the FeS after reaction2Thin-film material.
Embodiment 8
First, use Low Pressure Chemical Vapor Deposition on 4.5 inches of quartzy thin slice deposit thickness for's
Al2O3As dielectric layer, then using electron beam evaporation deposition method in obtained Al2O3/SiO2Continue deposit thickness on substrate
ForIron thin film, as plating iron predecessor.
Then, the plating iron predecessor is positioned over to the downstream of tube furnace, the upstream of tube furnace is placed with aluminium oxide ceramics earthenware
Crucible, and 1.55 grams of sulphur powder are added, boiler tube external application silica gel heating band parcel, and connect temperature control device.Afterwards, lead to tube furnace
Enter argon gas, speed 80sccm, as shown in Figure 1.Tube furnace, when tube furnace is raised to 180 DEG C, is opened with 14 DEG C/min of heatings
Heating tape, makes the sulphur powder in crucible be warming up to 155 DEG C, sulphur powder is evaporated to sulfur gas, and is managed as argon gas enters
The downstream of formula stove.
After 55 minutes, tube furnace rises to 280 DEG C with 11 DEG C/min of programming rate, keep temperature carry out reaction 8 it is small when,
It is FeS by iron thin film vulcanization2, that is, obtain the FeS2Thin-film material.After reaction, close and remove heating tape, wait tube furnace
Room temperature is naturally cooling to, tube furnace is opened and takes out the FeS after reaction2Thin-film material.
Fig. 2 and Fig. 3 is the FeS of 1-3 of the embodiment of the present invention2The XRD spectrum of thin-film material and Raman collection of illustrative plates, it was demonstrated that use
The preparation method that the present invention limits can grow brilliant as purer FeS2。
Table 1 is FeS of the prior art2The FeS of thin-film material and 1-8 of the embodiment of the present invention2The electric property of thin-film material
Contrast
The prior art includes sol-gal process chemical synthesis FeS2, sulfidation-oxidation iron thin film, magnetron sputtering FeS2Deng.Its
In, FeS that sol-gel chemistries synthetic method obtains2Film quality is preferable, but mobility is relatively low, often below 1cm2V-1s-1；
The method relative mobility of sulfidation-oxidation iron thin film is higher, but sulfidation-oxidation iron thin film needs to use H2S, and H2S can corrosion tester
Device, while not environmentally.Magnetron sputtering FeS2Although simple, FeS2Target is more expensive, is not appropriate for using on a large scale.
FeS provided by the invention2Thin-film material uses and first deposits iron thin film, then it is FeS to be vulcanized2The method system of film
Standby to obtain, the preparation method is simple, and cost is low, and obtained FeS2The crystalline substance of thin-film material is high as purity, can adjust and fit
A variety of environment and condition are answered, has potential application to scientific research and other large-scale productions aspects.The preparation method
Feasibility is high, preparation method is simple, production cost is low, is easy to industrialized mass production, while the FeS prepared2Film material
Material can be widely applied in various electronics, energy field.
Those of ordinary skills in the art should understand that：The discussion of any of the above embodiment is exemplary only, not
It is intended to imply that the scope of the present disclosure (including claim) is limited to these examples；Under the thinking of the present invention, above example
Or can also be combined between the technical characteristic in different embodiments, and there is different aspect present invention as described above
Many other changes, in order to it is concise they do not provided in details.Therefore, within the spirit and principles of the invention,
Any omission for being made, modification, equivalent substitution, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
- A kind of 1. FeS2The preparation method of thin-film material, it is characterised in that comprise the following steps：1) dielectric layer on silicon sheet or quartzy thin slice；2) continue to deposit iron thin film on the dielectric layer again, obtain plating iron predecessor；3) the plating iron predecessor is positioned over to the downstream of heating furnace, sulphur is positioned over to the upstream of heating furnace, is led to heating furnace Entering inert gas, sulphur is heated to 130~180 DEG C, sulphur is evaporated to sulfur gas, and as inert gas enters heating furnace Downstream；4) heating furnace is risen into reaction temperature with 5~25 DEG C/min of programming rate, keeps temperature to be reacted, by iron thin film Vulcanize as FeS2, that is, obtain the FeS2Thin-film material；The inert gas is selected from argon gas, nitrogen；The reaction temperature of the heating furnace is 200~800 DEG C.
- 2. FeS according to claim 12The preparation method of thin-film material, it is characterised in that in the step 1), use At least one of Low Pressure Chemical Vapor Deposition, sputtering method and plasma deposition processes method by dielectric layer deposition in silicon sheet or On quartzy thin slice.
- 3. FeS according to claim 22The preparation method of thin-film material, it is characterised in that the thickness of the dielectric layer is
- 4. FeS according to claim 22The preparation method of thin-film material, it is characterised in that the dielectric material of the dielectric layer Material is selected from SiO2, Al2O3, ZrO2And HfO2At least one of.
- 5. FeS according to claim 12The preparation method of thin-film material, it is characterised in that in the step 2), use At least one of electron beam evaporation deposition method and sputtering method method continue to deposit iron thin film on the dielectric layer.
- 6. FeS according to claim 52The preparation method of thin-film material, it is characterised in that the thickness of the iron thin film is
- 7. FeS according to claim 12The preparation method of thin-film material, it is characterised in that the flow velocity of the inert gas For 20~500sccm.
- 8. FeS according to claim 12The preparation method of thin-film material, it is characterised in that in the step 4), reaction When time is 2~8 small.
- A kind of 9. FeS2Thin-film material, it is characterised in that the FeS2Thin-film material is according to any one institute in claim 1~8 The FeS stated2The preparation method of thin-film material is made.
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| CN102337524B (en) * | 2010-07-20 | 2013-07-17 | 中国科学院上海硅酸盐研究所 | Preparation method of Bi-based chalcogenide thermoelectric thin film |
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