CN107622949B - A method of black phosphorus two-dimensional material is prepared based on plasma immersion injection technique - Google Patents
A method of black phosphorus two-dimensional material is prepared based on plasma immersion injection technique Download PDFInfo
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- CN107622949B CN107622949B CN201710728776.9A CN201710728776A CN107622949B CN 107622949 B CN107622949 B CN 107622949B CN 201710728776 A CN201710728776 A CN 201710728776A CN 107622949 B CN107622949 B CN 107622949B
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- black phosphorus
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- dimensional material
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Abstract
The present invention provides a kind of method for preparing black phosphorus two-dimensional material based on plasma immersion injection technique, corrasion is generated to black phosphorus crystal material using the hydrogen plasma that plasma immersion injected system generates, to get the controllable black phosphorus two-dimensional material of the number of plies；Then it recycles acetylene plasma to carry out depositing/doping treatment to black phosphorus two-dimensional material, improves stability of the black phosphorus two-dimensional material under room temperature, air environment；This method not only increases the total quality of black phosphorus two-dimensional material, while also simplifying the technique of preparation, realizes from black phosphorus crystal to the integrated preparation flow for stablizing black phosphorus two-dimensional material.
Description
Technical field
It is specifically a kind of that black phosphorus is prepared based on plasma immersion injection technique the present invention relates to molecular material technical field
The method of two-dimensional material.
Background technique
Black phosphorus has excellent electron mobility and direct band gap structure as a kind of New Two Dimensional material, and the number of plies is got over
Few, band-gap energy is bigger, can be widely used in the fields such as field effect transistor, photoelectric cell, solar battery.
Currently, the method for prior art preparation black phosphorus two-dimensional material is mainly mechanical stripping method and liquid phase stripping method.Pass through
The two-dimensional material randomness that these methods are prepared is larger, and uniformity is poor, and the integrality and the number of plies of material are unable to control, it is also necessary to
It is subsequent carry out according to demand centrifugation or screening operation can use, increase the complexity of preparation process.In addition, black phosphorus two dimension material
Expect that property is unstable, is easy to react with oxygen gas and water etc., which increases difficulty prepared by black phosphorus two-dimensional material.
Plasma immersion injection technique is a kind of new technique for combining plasma immersion and ion implanting and using.
During processing, sample is immersed in plasma atmosphere always, by the influence of back bias voltage, allows plasma bombardment sample
Surface not only can implant ions on sample, and can also sample surfaces be performed etching with effect.Because plasma soaks
Do not have the unique advantage of injection technique, is widely used in the surface treatment of various types of materials.
(application number 201510475008.8 uses oxygen plasma etch black phosphorus two-dimensional material body to Chinese patent literature
Processing method) a kind of processing method using oxygen plasma etch black phosphorus two-dimensional material body is disclosed, which utilizes inductance
Coupled plasma etch system performs etching the black phosphorus material of multilayer and achievees the purpose that material is thinned, while generating first
Then layer phosphorous oxide protective layer re-forms the second layer on thinned black phosphorus two-dimensional material surface by atomic layer deposition coating system
Aluminum oxide film protective layer.However, in the invention, the phosphorous oxide protective layer of black phosphorus two-dimensional material Surface Creation is very unstable,
It easily reacts with the water in air, and further increases difficulty and cost that other protective layers increase operation, it is unfavorable
In industrial application.
Summary of the invention
Aiming at the problems existing in the prior art, the object of the present invention is to provide one kind injects skill based on plasma immersion
The method that art prepares black phosphorus two-dimensional material.
To achieve the goals above, the invention adopts the following technical scheme:
A method of black phosphorus two-dimensional material being prepared based on plasma immersion injection technique, comprising the following steps: pass through
Plasma immersion injection technique, using plasma perform etching reaction to black phosphorus crystal material, obtain controllable black of the number of plies
Phosphorus two-dimensional material, wherein the plasma is hydrogen plasma or inert gas plasma.Preferably, the indifferent gas
Bulk plasmon is He plasma, Ar plasma etc..
It is preferably further comprising the steps of in order to further increase the stability of black phosphorus two-dimensional material, pass through plasma
Submerge deposition or injection that injection technique carries out carbon to the black phosphorus two-dimensional material.
Preferably, the etching reaction is that hydrogen or inert gas by plasma producing apparatus generate hydrogen plasma
Or inert gas plasma, back bias voltage effect under so that ion formed between plasma and black phosphorus crystal surface from
In black phosphorus crystal material surface black phosphorus crystal is constantly thinned, to obtain black phosphorus two in vertical bombardment after being accelerated in sub- sheaths
Tie up material.
Preferably, the deposition of the carbon or injection are that acetylene or methane by plasma producing apparatus generate acetylene
Plasma or methane plasma, under back bias voltage effect, so that ion is between plasma and black phosphorus two-dimensional material surface
It is accelerated in the ion sheath of formation, then acts perpendicularly to black phosphorus two-dimensional material, and then carbon is made to be deposited on black phosphorus two dimension
Material surface and/or carbon are mixed in black phosphorus two-dimensional material.
Bombardment intensity can be effectively controlled by parameter regulations such as negative bias Compressive Strength and action times, to realize black phosphorus material
The controllability of bed of material number.
It is further preferred that the flow that hydrogen or inert gas are passed through plasma producing apparatus is 10-500sccm, it is excellent
100-200sccm, air pressure 0.1-0.5Pa are selected, hydrogen or inert gas are ionized using radio frequency, radio-frequency power is 20W or more, excellent
30-500W, more preferable 50-350W are selected, pulsed bias is -500~-10V, preferably -200~-10V, etch period 5-
40min, preferably 10-20min.
It is further preferred that the flow that acetylene or methane pass through plasma producing apparatus is 10-200sccm, preferably 40-
100sccm, air pressure 0.1-0.5Pa ionize acetylene or methane, radio-frequency power 30-500W using radio frequency, and Dc bias is-
100~-10V, preferably -500~-10V, action time 5-15min.
It is black the present invention relates to providing a kind of based on plasma immersion injection technique and preparing specifically, in one aspect
The method of phosphorus two-dimensional material specifically includes following steps (schematic diagram of its device therefor is as shown in Figure 1):
(1) black phosphorus crystal is transferred to silica/silicon piece surface or silicon nitride/silicon chip surface, and impregnated in acetone,
It is heated to 30-70 DEG C, preferably 50 DEG C, impregnates 20-60min, preferably 30min removes the impurity on surface, obtains sample 1；
(2) sample 1 is put on the target platform 2 in plasma immersion injection device；
(3) it vacuumizes, until the vacuum degree in vacuum cavity 3 is 4 × 10-3Pa-6×10-3Pa；It is preferred that 5 × 10-3Pa。
(4) it is passed through hydrogen or inert gas, opens plasma producing apparatus, the flow of hydrogen or inert gas is 10-
500sccm, preferably 100-200sccm, air pressure 0.1-0.5Pa ionize hydrogen using radio frequency or inert gas, radio-frequency power are
20W or more, preferably 30-500W, more preferable 50-350W, pulsed bias be -500~-10V, preferably -200~-10V, generation
Hydrogen plasma or inert gas plasma start to perform etching black phosphorus crystal effect, etch period 5-40min, preferably
10-20min obtains black phosphorus two-dimensional material.
On the other hand, the invention further relates to provide one kind to prepare black phosphorus two based on plasma immersion injection technique
The method for tieing up material, specifically includes the following steps:
(1) black phosphorus crystal is transferred to silica/silicon piece surface, and impregnated in acetone, be heated to 30-70 DEG C, preferably
50 DEG C, 20-60min is impregnated, preferably 30min removes the impurity on surface, obtains sample 1；
(2) sample 1 is put on the target platform 2 in plasma immersion injection device；
(3) it vacuumizes, until the vacuum degree in vacuum cavity 3 is 4 × 10-3Pa-6×10-3Pa；It is preferred that 5 × 10-3Pa；
(4) it is passed through hydrogen or inert gas, opens plasma producing apparatus, the flow of hydrogen or inert gas is 10-
500sccm, preferably 100-200sccm, air pressure 0.1-0.5Pa ionize hydrogen using radio frequency or inert gas, radio-frequency power are
20W or more, preferably 30-500W, more preferable 50-350W, pulsed bias be -500~-10V, preferably -200~-10V, generation
Hydrogen plasma or inert gas plasma start to perform etching black phosphorus crystal effect, etch period 5-40min, preferably
10-20min obtains black phosphorus two-dimensional material；
(5) it closes plasma producing apparatus and stops being passed through hydrogen or inert gas, change at being passed through acetylene or methane
Gas；
(6) acetylene or methane gas are passed through a period of time, after hydrogen or inert gas empty, reopen plasma
Generating device, acetylene or methane flow are 10-200sccm, preferably 40-100sccm, air pressure 0.1-0.5Pa, using radio frequency electrical
From acetylene or methane, radio-frequency power 30-300W, Dc bias is -100~-10V, preferably -500~-10V, the acetylene of generation
Plasma or methane plasma act on black phosphorus two-dimensional material obtained in step (4), action time 5-15min,
Carbon is adulterated in black phosphorus two-dimensional material and/or deposits carbon on black phosphorus two-dimensional material surface, and then obtains stable black phosphorus
Two-dimensional material.
Another aspect, the present invention provide a kind of black phosphorus two-dimensional material, are to be injected by above-mentioned based on plasma immersion
What the method that technology prepares black phosphorus two-dimensional material was prepared, doped with carbon and/or described in the black phosphorus two-dimensional material
Black phosphorus two-dimensional material surface is deposited with carbon.
To sum up, using plasma submergence injection technique of the present invention prepares the black phosphorus two-dimensional material having good stability.Wherein,
Discharge process is carried out to injection hydrogen or inert gas by plasma immersion injected system and generates hydrogen plasma or inertia
Gaseous plasma, so that black phosphorus crystal material is in gas ions atmosphere on target platform.Then, in back bias voltage environment, due to
The effect of electric field, ion are accelerated in the ion sheath that plasma and black phosphorus crystal surface are formed, hydrogen plasma or lazy
Property gaseous plasma vertically bombard black phosphorus crystal surface, on target platform black phosphorus crystal generate corrasion, be constantly thinned black
The thickness of phosphorus crystal, wherein intensity is bombarded by adjusting the state modulators such as negative bias Compressive Strength and action time, to obtain the number of plies
Controllable black phosphorus two-dimensional material.Then, optionally the hydrogen or inert gas that inject in plasma immersion injected system are changed into
Other gases (such as acetylene or methane) adjust back bias voltage and power parameter, are made using plasma to the modified of material surface
With, protective film is formed in the few layer of black phosphorus two-dimensional material surface doping carbon and/or deposition carbon of acquisition, it can be effectively
The stability for enhancing black phosphorus two-dimensional material, extends its holding time under normal temperature air environment.
Beneficial effects of the present invention
1, using plasma submergence injection technique of the present invention prepares black phosphorus two-dimensional material, can obtain large stretch of and integrality
Preferable black phosphorus two-dimensional material；
2, by the setting of relevant parameter, the number of plies of black phosphorus two-dimensional material can be accurately controlled；
3, by changing relevant parameter and working gas, black phosphorus two-dimensional material can be carried out depositing/doping treatment, improved
Stability of the black phosphorus two-dimensional material in normal temperature air environment；
4, the present invention on the same device, realizes and the mesh for stablizing black phosphorus two-dimensional material is thinned and obtained to black phosphorus crystal
, preparation method is simplified, preparation efficiency is high.
Detailed description of the invention
Fig. 1 is that plasma immersion injected system prepares black phosphorus two-dimensional material schematic diagram；
1- sample, 2- target platform, 3- vacuum cavity, 4- metal frame；
Fig. 2 a is the optical microscopy map of black phosphorus crystal before the hydrogen plasma process of embodiment 1；
Fig. 2 b is the AFM figure of black phosphorus crystal before the hydrogen plasma process of embodiment 1；
Fig. 2 c is the thickness chart of black phosphorus crystal before the hydrogen plasma process of embodiment 1；
Fig. 2 d is the optical microscopy map of black phosphorus two-dimensional material after the hydrogen plasma process of embodiment 1；
Fig. 2 e is the AFM figure of black phosphorus two-dimensional material after the hydrogen plasma process of embodiment 1；
Fig. 2 f is the thickness chart of black phosphorus two-dimensional material after the hydrogen plasma process of embodiment 1；
It is aobvious that Fig. 3 (a) is that the black phosphorus two-dimensional material after hydrogen plasma process of embodiment 2 is exposed to the optics before air
Micro- figure；
Fig. 3 (b) is that the black phosphorus two-dimensional material after hydrogen plasma process of embodiment 2 is exposed to light after air 24 hours
Learn micrograph；
Fig. 3 (c) be embodiment 3 through hydrogen plasma+acetylene plasma, treated that black phosphorus two-dimensional material is exposed to
Optical microscopy map before air；
Fig. 3 (d) be embodiment 3 through hydrogen plasma+acetylene plasma, treated that black phosphorus two-dimensional material is exposed to
Optical microscopy map after air 24 hours.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be pointed out that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The present invention is further explained in the light of specific embodiments.
Embodiment 1
A method of black phosphorus two-dimensional material is prepared using plasma immersion injection technique, comprising the following steps:
(1) it will be transferred to silica/silicon piece surface with a thickness of the black phosphorus crystal of 97nm, and impregnates heating in acetone
To 50 DEG C, after impregnating 30min, the impurity on surface is removed, sample is obtained；
(2) sample is put on the target platform of plasma immersion injection device；
(3) it vacuumizes, until the vacuum degree in vacuum cavity is 5 × 10-3Pa；
(4) it is passed through hydrogen, opens plasma producing apparatus, the flow of hydrogen is 150sccm, and air pressure 0.15Pa is adopted
Hydrogen, radio-frequency power 200W are ionized with radio frequency, pulsed bias is -100V, and the hydrogen plasma of generation starts to black phosphorus crystal
Effect is performed etching, etch period 15min obtains the black phosphorus two-dimensional material with a thickness of 42nm.
Embodiment 2
A method of black phosphorus two-dimensional material is prepared using plasma immersion injection technique, comprising the following steps:
(1) it will be transferred to silica/silicon piece surface with a thickness of the black phosphorus crystal of 69nm, and impregnates heating in acetone
To 50 DEG C, after impregnating 30min, the impurity on surface is removed, sample is obtained；
(2) sample is put on the target platform of plasma immersion injection device；
(3) it vacuumizes, until the vacuum degree in vacuum cavity is 5 × 10-3Pa；
(4) it is passed through hydrogen, opens plasma producing apparatus, the flow of hydrogen is 150sccm, and air pressure 0.15Pa is adopted
Hydrogen, radio-frequency power 200W are ionized with radio frequency, pulsed bias is -120V, and the hydrogen plasma of generation starts to black phosphorus crystal
Effect is performed etching, etch period 15min obtains the black phosphorus two-dimensional material with a thickness of 16nm.
From Fig. 3 (a) and Fig. 3 (b) as can be seen that the black phosphorus two-dimensional material of this example after treatment is exposed to air 24
After hour, black phosphorus two-dimensional material surface stain.
Embodiment 3
A method of black phosphorus two-dimensional material is prepared using plasma immersion injection technique, comprising the following steps:
(1) it will be transferred to silica/silicon piece surface with a thickness of 80nm black phosphorus crystal, and with acetone soak, remove surface
Impurity, obtain sample；
(2) sample is put on the target platform in plasma immersion injection device；
(3) it vacuumizes, until the vacuum degree in vacuum cavity is 5 × 10-3Pa；
(4) it is passed through hydrogen, opens plasma producing apparatus, the flow of hydrogen is 150sccm, and air pressure 0.15Pa is adopted
Hydrogen, radio-frequency power 200W are ionized with radio frequency, pulsed bias is -100V, and the hydrogen plasma of generation starts to black phosphorus crystal
Effect is performed etching, etch period 20min obtains the black phosphorus two-dimensional material with a thickness of 15nm；
(5) it closes plasma producing apparatus and stops hydrogen and be passed through, change at being passed through acetylene gas；
(6) acetylene gas is passed through a period of time, after hydrogen emptying, reopens plasma producing apparatus, acetylene stream
Amount is 60sccm, air pressure 0.2Pa, ionizes acetylene, radio-frequency power 50W using radio frequency, Dc bias is -25V, the second of generation
Alkynes plasma starts to act on black phosphorus two-dimensional material obtained in step (4), action time 10min, in black phosphorus two dimension material
Carbon is adulterated in material and/or deposits carbon on black phosphorus two-dimensional material surface, and then obtains stable black phosphorus two-dimensional material.
From Fig. 3 (c) and (d) as can be seen that the treated black phosphorus two-dimensional material of the present embodiment is exposed to air 24 is small
Shi Hou, black phosphorus two-dimensional material do not change, and illustrate that its is highly stable.
Above-described embodiment is only intended to clearly illustrate the invention example, and not has to the invention
The restriction of body embodiment.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all of the invention
Guarantor of any obvious changes or variations extended out within spirit and principle still in the invention claim
It protects among range.
Claims (8)
1. a kind of method for preparing black phosphorus two-dimensional material based on plasma immersion injection technique, which is characterized in that including following
Step: by plasma immersion injection technique, using plasma performs etching reaction to black phosphorus crystal material, obtains the number of plies
Controllable black phosphorus two-dimensional material, the plasma are hydrogen plasma or inert gas plasma；
Wherein, further comprising the steps of, carbon is carried out to the black phosphorus two-dimensional material by plasma immersion injection technique
Deposition or injection；
The deposition of the carbon or injection be acetylene or methane by plasma producing apparatus generate acetylene plasma or
Methane plasma acts on black phosphorus two-dimensional material, makes that carbon is deposited on black phosphorus two-dimensional material surface and/or carbon is mixed
In black phosphorus two-dimensional material.
2. the method according to claim 1 for preparing black phosphorus two-dimensional material based on plasma immersion injection technique, special
Sign is that hydrogen or inert gas are by plasma producing apparatus generation plasma, and wherein hydrogen or inert gas are passed through
The flow of plasma producing apparatus is 10-500sccm, air pressure 0.1-0.5Pa；Using radio frequency ionized gas, radio-frequency power
For 30-500W；Pulsed bias is -500~-10V.
3. the method according to claim 1 for preparing black phosphorus two-dimensional material based on plasma immersion injection technique, special
Sign is, etch period 5-40min.
4. the method according to claim 1 for preparing black phosphorus two-dimensional material based on plasma immersion injection technique, special
Sign is that the controllable black phosphorus two-dimensional material of the number of plies can be few layer.
5. the method according to claim 1 for preparing black phosphorus two-dimensional material based on plasma immersion injection technique, special
Sign is that the flow that acetylene or methane pass through plasma producing apparatus is 10-200sccm；Air pressure is 0.1-0.5Pa, is used
Radio frequency ionizes acetylene or methane, radio-frequency power 30-500W, and Dc bias is -100~-10V.
6. the method according to claim 5 for preparing black phosphorus two-dimensional material based on plasma immersion injection technique, special
Sign is that the action time of acetylene or methane plasma is 5-15min.
7. the method according to claim 1 for preparing black phosphorus two-dimensional material based on plasma immersion injection technique, special
Sign is that the black phosphorus crystal material is placed on silica/silicon piece or silicon nitride/silicon chip surface before etching, and is impregnated
In acetone, it is heated to 30-70 DEG C, impregnates 20-60min, clean the surface impurity.
8. a kind of black phosphorus two-dimensional material, which is characterized in that be by of any of claims 1-7 based on plasma
What the method that submergence injection technique prepares black phosphorus two-dimensional material was prepared, doped with carbon in the black phosphorus two-dimensional material
And/or black phosphorus two-dimensional material surface is deposited with carbon.
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| US8343860B1 (en) * | 2010-03-23 | 2013-01-01 | L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | High C content molecules for C implant |
| CN106315531A (en) * | 2016-08-23 | 2017-01-11 | 深圳先进技术研究院 | Black phosphorus modified by aromatic compound and preparation method and application thereof |
| CN106384719A (en) * | 2015-08-06 | 2017-02-08 | 王贝贝 | Processing method of using oxygen plasma to etch black-phosphorus two-dimensional material body |
| KR20170072806A (en) * | 2015-12-17 | 2017-06-27 | 고려대학교 산학협력단 | Apparatus for etching thickness of black phosphorous |
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2017
- 2017-08-23 CN CN201710728776.9A patent/CN107622949B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8343860B1 (en) * | 2010-03-23 | 2013-01-01 | L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | High C content molecules for C implant |
| CN106384719A (en) * | 2015-08-06 | 2017-02-08 | 王贝贝 | Processing method of using oxygen plasma to etch black-phosphorus two-dimensional material body |
| KR20170072806A (en) * | 2015-12-17 | 2017-06-27 | 고려대학교 산학협력단 | Apparatus for etching thickness of black phosphorous |
| CN106315531A (en) * | 2016-08-23 | 2017-01-11 | 深圳先进技术研究院 | Black phosphorus modified by aromatic compound and preparation method and application thereof |
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| Plasma-Treated Thickness-Controlled Two-Dimensional Black Phosphorus and Its Electronic Transport Properties;Jingyuan Jia et al;《ACS NANO》;20150824;正文第1-18页 * |
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