阅读说明：本技术 一种大面积薄层二维碲烯的制备方法 (A kind of preparation method of large area thin layer two dimension tellurium alkene ) 是由 郑晶莹 江凡 詹红兵 陈奇俤 于 2019-09-30 设计创作，主要内容包括：本发明提供了一种大面积薄层二维碲烯的制备方法,该制备方法包括以下过程：以碲粉末为碲源,通过将碲粉磨细并取少量以2-4列形式放置在SiO<Sub>2</Sub>/Si基底上,每列间相隔约2-4 mm,在此基底上再覆盖另一SiO<Sub>2</Sub>/Si基底,构建限域生长空间,放置于单温管式炉中,在700-800℃下退火10-40 min,碲蒸发进入气相,大部分停留在限域空间内,直接在基底上实现大面积的生长。该方法制备出来的碲烯薄膜具有生长面积大、厚度薄、较为均匀等优点。(The present invention provides a kind of preparation methods of large area thin layer two dimension tellurium alkene, which includes following procedure: using telloy as tellurium source, by tellurium grinding is thin and take and be placed on SiO in the form of 2-4 column on a small quantity 2 In/Si substrate, about 2-4 mm is separated by between each column, covers another SiO again in this substrate 2 / Si substrate constructs confinement growing space, is placed in single warm tube furnace, and anneal 10-40 min at 700-800 DEG C, and tellurium evaporates into gas phase, largely rests in confinement space, and the growth of large area is realized directly in substrate.The tellurium alkene film that this method prepares has many advantages, such as that growth area is big, thickness is thin, more uniform.)

1. a kind of preparation method of large area thin layer two dimension tellurium alkene, it is characterised in that: the following steps are included:

(1) a small amount of tellurium powder is taken to be fully ground in mortar

(2) ground tellurium powder is taken and is placed on SiO on a small quantity₂In/Si substrate, 2-4 column are positioned to, then place another SiO₂/Si Substrate is covered on tellurium powder；

(3) tellurium powder/substrate-loading in step (2) is then placed on tube furnace center in cleaned quartz boat together Warm area carries out high annealing, and then obtains the thin layer two dimension tellurium alkene of large area.

2. preparation method according to claim 1, it is characterised in that: comprising the following specific steps

(1) it weighs 0.1 g tellurium powder to be fully ground in the agate mortar, until there is no granular sensation；

(2) 2 SiO are cut with silicon wafer knife₂/ Si substrate, every substrate sizes are the cm of 1.2 × 0.8-1.6 × 0.8, use nitrogen gun The stream of nitrogen gas of ejection removes substrate surface granule foreign, then successively cleans having for substrate surface using acetone, ethyl alcohol, isopropanol Machine pollutant weighs the tellurium powder of milled in 2-20 mg step (1), divides 2-4 column to be placed in substrate, another substrate is covered On tellurium powder；

(3) quartz boat is successively cleaned by ultrasonic to 10-15 min in ethyl alcohol, deionized water, by the two panels overlapping in step (2) Substrate is placed in quartz boat, and entire quartz boat is placed on the center warm area of tube furnace, and whole process carries out under argon atmosphere, argon gas Flow velocity is 100 sccm, is passed through 15 min of argon gas first to drain inner air tube, setting program is that 20 DEG C/min is warming up to 700- 800 DEG C, keep the temperature 10-40 min, subsequent Temperature fall opens fire door in 300 DEG C and following temperature, be cooled to 70 DEG C and Argon gas is closed below and takes out sample.

3. preparation method according to claim 1 or 2, it is characterised in that: adjacent two column tellurium powder interval 2-4 in step (2) Mm, two panels substrate polish face are staggered relatively.

Technical field

The invention belongs to the preparation fields of dimensional thinlayer material, and in particular to a kind of preparation of large area thin layer two dimension tellurium alkene Method.

Background technique

Tellurium alkene becomes the New Two Dimensional material being concerned because having unique band structure and material property in recent years. This materials band structure shows strong number of plies dependence, and single layer tellurium alkene has indirect band gap structure, band gap size ~ 1 EV, and body block tellurium then has the indirect band gap of ~ 0.35 eV.In addition, tellurium also shows many excellent properties, moved Ru higher Shifting rate and on-off ratio and good photoconductivity, pyroelectricity, nonlinear optical response and stability etc., in sensor, electronics Device and catalytic field show huge application prospect.

The key of tellurium alkene functionization is promoted to be to realize the controllable preparation of large-area two-dimensional tellurium alkene film.Prepare tellurium alkene method Mainly including crystal stripping method, solvent-thermal process method, physical vapour deposition (PVD), molecular beam epitaxy etc., but above method system at present There is the problems such as number of plies is difficult to control, lateral dimension is smaller in standby obtained tellurium alkene, therefore the present invention mainly passes through improvement routine Physical vaporous deposition, propose confinement space in deposit method, it is thin that the uniform two-dimentional tellurium alkene of large area, the number of plies is prepared Film.

Summary of the invention

It is an object of the invention to overcome the shortcomings of art methods, with a kind of novel confinement physical vapour deposition (PVD) side Method realizes the preparation of large-area two-dimensional tellurium alkene, and the preparation process is easy easily to be implemented, and the area of the tellurium alkene film of acquisition is larger, can Up to 1-3 mm², application suitable for electronic device etc..

For achieving the above object, the present invention adopts the following technical scheme:

A kind of preparation method of large area thin layer two dimension tellurium alkene, comprising the following steps:

(1) a small amount of tellurium powder is taken to be fully ground in mortar

(2) ground tellurium powder is taken and is placed on SiO on a small quantity₂In/Si substrate, 1-4 column are positioned to, then place another SiO₂/ Si substrate is covered on tellurium powder；

(3) tellurium powder/substrate-loading in step (2) is then placed on tube furnace center in cleaned quartz boat together Warm area carries out high annealing, and then obtains the thin layer two dimension tellurium alkene of large area.

Specific step is as follows:

(1) 0.1 g tellurium powder is weighed to be fully ground in the agate mortar to no granular sensation；

(2) 2 SiO are cut with silicon wafer knife₂/ Si substrate, about 1.2 × 0.8-1.6 × 0.8 cm of every substrate sizes, uses nitrogen The stream of nitrogen gas that rifle sprays removes substrate surface granule foreign, then successively cleans substrate surface using acetone, ethyl alcohol, isopropanol Organic pollutant weighs the tellurium powder of milled in 2-20 mg step (1), divides 2-4 column to be placed in substrate, another substrate is covered It covers in the substrate for being placed with powder；

(3) quartz boat is successively cleaned by ultrasonic in ethyl alcohol, deionized water to 10-15 min, is used after drying, it will be in step (2) Two panels overlapping substrate be placed in quartz boat, entire quartz boat is placed on the center warm area of tube furnace, SiO₂/ Si substrate pair The thermocouple of true centric warm area, whole process carry out under argon atmosphere, and argon gas flow velocity is 100 sccm, are passed through 15 min of argon gas To drain inner air tube, setting program is that 20 DEG C/min is warming up to 700-800 DEG C, keeps the temperature 10-40 min, then drops naturally Temperature is cooled to 70 DEG C or less closing argon gas and takes out sample in 300 DEG C or less opening fire doors.

Adjacent two column tellurium powder interval about 2-4 mm in step (2), two panels substrate polish face is staggered relatively, upper layer base length Slightly larger than lower substrate, the thermocouple for the substrate centring warm area placed on quartz boat.

Remarkable advantage of the invention is:

The present invention is based on physical vaporous depositions, using the growing environment of two panels substrate building space confinement staggered relatively, with molten The lower tellurium powder of point is tellurium source and is directly placed in confinement space, be higher than tellurium fusing point at a temperature of, can be due to when tellurium gasifies The blocking of upper substrate and be largely limited in confinement space, the two-dimentional tellurium of large area thin layer is directly grown in substrate Alkene.The tellurium alkene growth that is configured to of confinement space creates more stable and controllable growing environment, and precursor concentration mentions in growth room High, flow velocity reduces, is evenly distributed, and is conducive to prepare uniform, the good tellurium alkene of crystallinity, the two-dimentional tellurium alkene area being prepared Up to 1-3mm², also, this method raw material are easy to get, and preparation process is simple, facilitates the performance and application study that promote tellurium alkene.

Detailed description of the invention

Fig. 1 is the optical microscope under synthesized 10 times of two-dimentional tellurium alkene；

Fig. 2 is the optical microscope under synthesized 40 times of two-dimentional tellurium alkene；

Fig. 3 is the corresponding Raman spectrum collection of Fig. 2；

Fig. 4 is optical microscope image a) and corresponding Raman mapping image b)；

Fig. 5 is position-raman scattering intensity 3-D image corresponding to Fig. 4.

Specific embodiment:

The present invention is further illustrated by the following examples, but protection scope of the present invention is not limited to following implementation Example.