CN103086374B - Method for preparing graphene fluoride by atomic layer deposition device - Google Patents
Method for preparing graphene fluoride by atomic layer deposition device Download PDFInfo
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- CN103086374B CN103086374B CN201310056762.9A CN201310056762A CN103086374B CN 103086374 B CN103086374 B CN 103086374B CN 201310056762 A CN201310056762 A CN 201310056762A CN 103086374 B CN103086374 B CN 103086374B
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Abstract
The invention discloses a method for preparing graphene fluoride by an atomic layer deposition device. The method mainly comprises the following steps of: placing graphene on a support frame of the atomic layer deposition device through a transfer base, enabling the graphene to enter the cavity of the atomic layer deposition device by evaporation of a fluorinating agent in a glass and metal conversion piece, and absorbing the fluorine atom by the graphene, thereby realizing controllable preparation of the graphene fluoride. The method is completely controllable in technological process, simple and convenient to operate, and especially suitable for large-scale industrial production of graphene fluoride; and the graphene fluoride prepared by the method has wide application foreground in the fields of nano electronic appliances, lubricating materials, high capacity lithium batteries, and so on.
Description
Technical field
The invention belongs to nano material preparing technical field, relate to a kind of method of utilizing apparatus for atomic layer deposition to prepare fluorinated graphene.
Background technology
Two dimension Graphene has the feature of electric charge fractionation, may be the suitable material of manufacturing the needed anyon element of quantum computer.Being embedded in chemical doping thing at Graphene may exert an influence to carrier mobility, and huge specific surface area makes it very responsive for environment around, and its unique two-dirnentional structure makes Graphene have broad application prospects in sensor field.Fluorinated graphene is introduced fluorine atom on Graphene surface, makes the surface of Graphene can reduce and strengthen the hydrophobicity of Graphene.Fluorinated graphene can be regarded as Graphene to be fluoridized by some or all of, the sp in graphite
2structure is by the some or all of sp that is transformed into
3structure, but still keep two-dimensional sheet structure, be called as two-dimentional fluorinated ethylene propylene as the thinnest isolator.Fluorinated graphene, as the equivalent material of Teflon, is just becoming the very important hot research object in one, the practical field of nano material.
Fluorinated graphene chemical stability is strong, has extremely excellent electric property and mechanical property, has bright application prospect in emerging energy fields such as nanometer micro interface, lubricant, solar cells.The main method of preparing at present fluorinated graphene is taking fluorinated graphene as raw material, and N-Methyl pyrrolidone is as intercalator, and high temperature ultrasonic processing can obtain a certain amount of fluorinated graphene.Wherein, fluorographite is a kind of novel material, belongs to graphite deep processed product, and its production technology is ripe.Because graphite is laminate structure, interlayer carbon atom spacing is 1.42, link together securely, and interlamellar spacing is 3.35 by covalent linkage, faint Van der Waals force is stacked it, thereby graphite layers is very easily inserted other heteroatomss formation graphite intercalation compounds.In the time that graphite layers inset is fluorine atom, the compound between graphite layers that can form is fluorographite.Utilize fluorinated graphene method prepared by fluorographite to have serious technical deficiency, the number of plies of the Graphene that supersound process obtains and proterties are difficult to control, and the degree of fluorination of Graphene is also can not fine adjustment.
At present, the number of plies determine, the controlled urgently development research of fluorinated graphene preparation method of degree of fluorination.Ald be by the pulse of gas phase presoma is alternately passed into reactor and on depositing base chemisorption reaction form a kind of technological method of deposited film.Ald (ALD) there is outstanding controllability from restricted and complementary composition and the thickness of this technology to film that causes, prepared film conformality is good, purity is high and even, the material that can deposit at present comprises: oxide compound, nitride, fluorochemical, metal, carbide, composite structure, sulfide, nano thin-layers etc., arouse widespread concern.Utilize Atomic layer deposition method to mix fluorine element at individual layer or multi-layer graphene surface uniform, can overcome the shortcoming of utilizing fluorographite to prepare fluorinated graphene completely, can ensure quality product and the production schedule of fluorinated graphene completely.
Summary of the invention
The object of this invention is to provide a kind of technical process completely controlled, the simple to operation apparatus for atomic layer deposition that utilizes is prepared the method for fluorinated graphene.
The method of utilizing apparatus for atomic layer deposition to prepare fluorinated graphene of the present invention, wherein apparatus for atomic layer deposition comprises: cavity, be placed in the bracing frame in cavity, glass metal bridgeware and carrier gas bottle, the Fen Er road, air outlet of carrier gas bottle, wherein a road the 1st valve is connected with an inlet mouth of cavity, another Lu Jing 2 valves are connected with the inlet mouth of glass metal bridgeware, the air outlet of glass metal bridgeware the 3rd valve is connected with another inlet mouth of cavity, the air outlet of cavity the 4th valve is connected with vacuum pump, and its preparation method comprises the following steps:
Step 1: have the Copper Foil of Graphene to be placed in caustic solution growth, until Copper Foil corrodes totally completely;
Step 2: use ultraviolet and ozone generator that the organic impurity on transfer substrate surface is processed clean, utilize transfer substrate step 1 to be swum in to parallel the picking up of Graphene on caustic solution surface;
Step 3: will clean in deionized water, ethanol and acetone successively with the transfer substrate of Graphene, and dry up with gas;
Step 4: by process through step 3 with on the parallel bracing frame that is placed on apparatus for atomic layer deposition reaction cavity of transfer substrate of Graphene, get in the glass metal bridgeware that 5～50g fluorizating agent is placed on apparatus for atomic layer deposition;
Step 5: keeping reaction cavity temperature is 250 DEG C, and open vacuum pump, utilize vacuum pump by the vacuum degree control of reaction cavity in 1mTorr, close the 1st～the 4 four valve;
Step 6: open the 1st and the 4th valve, pass into the carrier gas that flow is 10～100sccm in cavity, move after 1～10 minute and open the 2nd valve, pass into the carrier gas that flow is 1～20sccm in glass metal bridgeware, the time was 10 ~ 90 seconds;
Step 7: close the 1st, the 2nd and the 4th valve, open the 3rd valve, close the 3rd valve after 15 seconds;
Step 8: the step 6 that reruns and step 7, circulate after 10～100 times, take out the transfer substrate on bracing frame, obtain fluorinated graphene.
In the present invention, described caustic solution can be that concentration is the FeCl of 0.1 ~ 2.0 mol/L
3, Fe (NO
3)
3or Fe
2(SO4)
3solution; Described transfer substrate can be silicon substrate, silicon nitride substrate or silicon dioxide substrates.Described fluorizating agent is xenon difluoride, tetrafluoro-methane or hydrogen fluoride.
In preparation process of the present invention, the carrier gas described in the gas described in step 3 and step 6, step 7 is nitrogen, helium or the argon gas of purity more than 99.999%.
Beneficial effect of the present invention: the present invention utilizes apparatus for atomic layer deposition to prepare fluorinated graphene, technical process is completely controlled, simple to operation, be particularly suitable for the large-scale industrial production of fluorinated graphene, the fluorinated graphene of preparation is with a wide range of applications in fields such as nano electron device, lubricant, high-capacity lithium batteries.
Brief description of the drawings
Fig. 1 is apparatus for atomic layer deposition schematic diagram;
In figure: 1. cavity, 2. bracing frame, 3. glass metal bridgeware, 4. carrier gas bottle, 5. the 1st valve, 6. the 2nd valve, 7. the 3rd valve, 8. the 4th valve, 9. vacuum pump, 10. Graphene, 11. transfer substrate.
Fig. 2 is the fluorinated graphene Raman collection of illustrative plates of preparation;
Fig. 3 is fluorinated graphene SEM image;
Fig. 4 is the various element EDS of fluorinated graphene image;
Fig. 5 is element distribution per-cent in fluorinated graphene.
Embodiment
The present invention prepares the apparatus for atomic layer deposition of fluorinated graphene and sees Fig. 1, this device comprises: cavity 1, be placed in the bracing frame 2 in cavity, glass metal bridgeware 3 and carrier gas bottle 4, the Fen Er road, air outlet of carrier gas bottle 4, wherein a road the 1st valve 5 is connected with an inlet mouth of cavity, another Lu Jing 2 valves 6 are connected with the inlet mouth of glass metal bridgeware, the air outlet of glass metal bridgeware the 3rd valve 7 is connected with another inlet mouth of cavity, and the air outlet of cavity the 4th valve 8 is connected with vacuum pump 9.In figure, 10 is Graphene, and 11 is transfer substrate.
Embodiment 1: utilize xenon difluoride as fluorizating agent, silicon dioxide substrates is as transfer substrate, FeCl
3solution is prepared fluorinated graphene as caustic solution
1) growth there is is the Copper Foil of Graphene be placed on the FeCl of 1.0 mol/L
3in solution, corrode 6 hours;
2) use ultraviolet and ozone generator to process silicon dioxide substrates 5 minutes, remove the organic impurity of silicon dioxide substrates, utilize silicon dioxide substrates will swim in FeCl
3parallel the picking up of Graphene in solution;
3) will in deionized water, ethanol and acetone, clean respectively 10 minutes successively with the silicon dioxide substrates of Graphene, and dry up with the nitrogen that purity is 99.999%;
4), by the parallel silicon dioxide substrates bracing frame that is placed on apparatus for atomic layer deposition reaction cavity inside, get 20g xenon difluoride particle and be placed in glass metal bridgeware; Keeping reaction cavity temperature is 250 DEG C, and opens vacuum pump, utilize vacuum pump by the vacuum degree control of reaction cavity at 1mTorr, close the 1st～4th valve;
5) open the 1st, the 4th valve, be the nitrogen that the purity of 40sccm is 99.999% to passing into flow in cavity, moving after 5 minutes, open the 2nd valve, is the nitrogen that the purity of 10sccm is 99.999% to passing into flow in glass metal bridgeware, after 30 seconds, close the 1st, the 2nd and the 4th valve, open the 3rd valve, after 15 seconds, close the 3rd valve, after step 5) circular flow 25 times, take out the silicon dioxide substrates on bracing frame, obtain fluorinated graphene.
The present invention provides fluorizating agent to reaction cavity at regular time and quantity, makes the fluorination process of Graphene completely controlled.As shown in Figure 2, wherein D peak, G peak, 2D peak, G ' peak-to-peak position are respectively 1368cm to the fluorinated graphene Raman collection of illustrative plates of this example preparation
-1, 1586cm
-1, 2706cm
-1and 2920cm
-1, D peak is suitable with G peak-to-peak value, illustrates that Graphene fluoridizes; As shown in Figure 3, in figure, fluorinated graphene contrast in silicon dioxide substrates is obvious for fluorinated graphene SEM image; The various element EDS of the fluorinated graphene image in the whole region of Fig. 3 as shown in Figure 4, shows in figure that the fluorine element content of fluorinated graphene is lower; In fluorographite, element distribution per-cent as shown in Figure 5, shows in figure that Graphene fluoridizes mass percent and the atomic percent of rear fluorine element and all exceed 3.5%.
Embodiment 2: utilize tetrafluoro-methane as fluorizating agent, silicon substrate is as transfer substrate, Fe (NO
3)
3solution is prepared fluorinated graphene as caustic solution
1) growth there is is the Copper Foil of Graphene be placed on the Fe (NO of 1.5 mol/L
3)
3in solution, corrode 6 hours;
2) use ultraviolet and ozone generator to process silicon substrate 5 minutes, remove the organic impurity of silicon substrate, utilize silicon substrate will swim in Fe (NO
3)
3parallel the picking up of Graphene in solution;
3) will in deionized water, ethanol and acetone, clean respectively 10 minutes successively with the silicon substrate of Graphene, and dry up with the helium that purity is 99.999%;
4), by the parallel silicon substrate bracing frame that is placed on apparatus for atomic layer deposition reaction cavity inside, get 20g tetrafluoro-methane particle and be placed in glass metal bridgeware; Keeping reaction cavity temperature is 250 DEG C, and opens vacuum pump, utilize vacuum pump by the vacuum degree control of reaction cavity at 1mTorr, close the 1st～4th valve;
5) open the 1st, the 4th valve, be the helium that the purity of 50sccm is 99.999% to passing into flow in cavity, moving after 5 minutes, open the 2nd valve, is the helium that the purity of 15sccm is 99.999% to passing into flow in glass metal bridgeware, after 30 seconds, close the 1st, the 2nd and the 4th valve, open the 3rd valve, after 15 seconds, close the 3rd valve, after step 5) circular flow 25 times, take out the silicon substrate on bracing frame, obtain fluorinated graphene.
Embodiment 3: utilize xenon difluoride as fluorizating agent, silicon nitride substrate is as transfer substrate, Fe
2(SO
4)
3solution is prepared fluorinated graphene as caustic solution
1) growth there is is the Copper Foil of Graphene be placed on the Fe of 0.5 mol/L
2(SO
4)
3in solution, corrode 8 hours;
2) use ultraviolet and ozone generator to process silicon nitride substrate 5 minutes, remove the organic impurity of silicon nitride substrate, utilize silicon nitride substrate will swim in Fe
2(SO
4)
3parallel the picking up of Graphene in solution;
3) will in deionized water, ethanol and acetone, clean respectively 10 minutes successively with the silicon nitride substrate of Graphene, and dry up with the argon gas that purity is 99.999%;
4), by the parallel silicon nitride substrate bracing frame that is placed on apparatus for atomic layer deposition reaction cavity inside, get 20g xenon difluoride particle and be placed in glass metal bridgeware; Keeping reaction cavity temperature is 250 DEG C, and opens vacuum pump, utilize vacuum pump by the vacuum degree control of reaction cavity at 1mTorr, close the 1st～4th valve;
5) open the 1st, the 4th valve, be the argon gas that the purity of 50sccm is 99.999% to passing into flow in cavity, moving after 5 minutes, open the 2nd valve, is the argon gas that the purity of 20sccm is 99.999% to passing into flow in glass metal bridgeware, after 30 seconds, close the 1st, the 2nd and the 4th valve, open the 3rd valve, after 15 seconds, close the 3rd valve, after step 5) circular flow 40 times, take out the silicon nitride substrate on bracing frame, obtain fluorinated graphene.
Embodiment 4: utilize xenon difluoride as fluorizating agent, silicon dioxide substrates is as transfer substrate, FeCl
3solution is prepared fluorinated graphene as caustic solution
1) growth there is is the Copper Foil of Graphene be placed on the FeCl of 1.5 mol/L
3in solution, corrode 5 hours;
2) use ultraviolet and ozone generator to process silicon dioxide substrates 5 minutes, remove the organic impurity of silicon dioxide substrates, utilize silicon dioxide substrates will swim in FeCl
3parallel the picking up of Graphene in solution;
3) will in deionized water, ethanol and acetone, clean respectively 10 minutes successively with the silicon dioxide substrates of Graphene, and dry up with the nitrogen that purity is 99.999%;
4), by the parallel silicon dioxide substrates bracing frame that is placed on apparatus for atomic layer deposition reaction cavity inside, get 5g xenon difluoride particle and be placed in glass metal bridgeware; Keeping reaction cavity temperature is 250 DEG C, and opens vacuum pump, utilize vacuum pump by the vacuum degree control of reaction cavity at 1mTorr, close the 1st～4th valve;
5) open the 1st, the 4th valve, be the nitrogen that the purity of 1sccm is 99.999% to passing into flow in cavity, moving after 1 minute, open the 2nd valve, is the nitrogen that the purity of 1sccm is 99.999% to passing into flow in glass metal bridgeware, after 10 seconds, close the 1st, the 2nd and the 4th valve, open the 3rd valve, after 15 seconds, close the 3rd valve, after step 5) circular flow 10 times, take out the silicon dioxide substrates on bracing frame, obtain fluorinated graphene.
Embodiment 5: utilize xenon difluoride as fluorizating agent, silicon dioxide substrates is as transfer substrate, FeCl
3solution is prepared fluorinated graphene as caustic solution
1) growth there is is the Copper Foil of Graphene be placed on the FeCl of 2.0 mol/L
3in solution, corrode 6 hours;
2) use ultraviolet and ozone generator to process silicon dioxide substrates 5 minutes, remove the organic impurity of silicon dioxide substrates, utilize silicon dioxide substrates will swim in FeCl
3parallel the picking up of Graphene in solution;
3) will in deionized water, ethanol and acetone, clean respectively 10 minutes successively with the silicon dioxide substrates of Graphene, and dry up with the nitrogen that purity is 99.999%;
4), by the parallel silicon dioxide substrates bracing frame that is placed on apparatus for atomic layer deposition reaction cavity inside, get 50g xenon difluoride particle and be placed in glass metal bridgeware; Keeping reaction cavity temperature is 250 DEG C, and opens vacuum pump, utilize vacuum pump by the vacuum degree control of reaction cavity at 1mTorr, close the 1st～4th valve;
5) open the 1st, the 4th valve, be the nitrogen that the purity of 100sccm is 99.999% to passing into flow in cavity, moving after 10 minutes, open the 2nd valve, is the nitrogen that the purity of 20sccm is 99.999% to passing into flow in glass metal bridgeware, after 90 seconds, close the 1st, the 2nd and the 4th valve, open the 3rd valve, after 15 seconds, close the 3rd valve, after step 5) circular flow 100 times, take out the silicon dioxide substrates on bracing frame, obtain fluorinated graphene.
Claims (5)
1. a method of utilizing apparatus for atomic layer deposition to prepare fluorinated graphene, wherein apparatus for atomic layer deposition comprises: cavity (1), be placed in the bracing frame (2) in cavity, glass metal bridgeware (3) and carrier gas bottle (4), the Fen Er road, air outlet of carrier gas bottle (4), wherein a road the 1st valve (5) is connected with an inlet mouth of cavity, another Lu Jing 2 valves (6) are connected with the inlet mouth of glass metal bridgeware, the air outlet of glass metal bridgeware the 3rd valve (7) is connected with another inlet mouth of cavity, the air outlet of cavity the 4th valve (8) is connected with vacuum pump (9), it is characterized in that preparation method comprises the following steps:
Step 1: have the Copper Foil of Graphene to be placed in caustic solution growth, until Copper Foil corrodes totally completely;
Step 2: use ultraviolet and ozone generator that the organic impurity on transfer substrate surface is processed clean, utilize transfer substrate step 1 to be swum in to parallel the picking up of Graphene on caustic solution surface;
Step 3: will clean in deionized water, ethanol and acetone successively with the transfer substrate of Graphene, and dry up with gas;
Step 4: by process through step 3 with on the parallel bracing frame that is placed on apparatus for atomic layer deposition reaction cavity of transfer substrate of Graphene, get in the glass metal bridgeware that 5～50g fluorizating agent is placed on apparatus for atomic layer deposition;
Step 5: keeping reaction cavity temperature is 250 DEG C, and open vacuum pump, utilize vacuum pump by the vacuum degree control of reaction cavity in 1mTorr, close the 1st～the 4 four valve;
Step 6: open the 1st and the 4th valve, pass into the carrier gas that flow is 10～100sccm in cavity, move after 1～10 minute and open the 2nd valve, pass into the carrier gas that flow is 1～20sccm in glass metal bridgeware, the time was 10～90 seconds; Step 7: close the 1st, the 2nd and the 4th valve, open the 3rd valve, close the 3rd valve after 15 seconds;
Step 8: the step 6 that reruns and step 7, circulate after 10～100 times, take out the transfer substrate on bracing frame, obtain fluorinated graphene.
2. the method for utilizing apparatus for atomic layer deposition to prepare fluorinated graphene according to claim 1, is characterized in that: described caustic solution is that concentration is FeCl3, Fe (NO3) 3 or Fe2 (SO4) 3 solution of 0.1～2.0mol/L.
3. the method for utilizing apparatus for atomic layer deposition to prepare fluorinated graphene according to claim 1, is characterized in that: described transfer substrate is silicon substrate, silicon nitride substrate or silicon dioxide substrates.
4. the method for utilizing apparatus for atomic layer deposition to prepare fluorinated graphene according to claim 1, is characterized in that: the carrier gas described in gas and step 6 described in step 3 is nitrogen, helium or the argon gas of purity more than 99.999%.
5. the method for utilizing apparatus for atomic layer deposition to prepare fluorinated graphene according to claim 1, is characterized in that: described fluorizating agent is xenon difluoride, tetrafluoro-methane or hydrogen fluoride.
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| EP2362459A1 (en) * | 2010-02-24 | 2011-08-31 | University College Cork-National University of Ireland, Cork | Modified graphene structure and method of manufacture thereof |
| CN102530910A (en) * | 2010-12-22 | 2012-07-04 | 海洋王照明科技股份有限公司 | Method for preparing fluorinated graphene |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2362459A1 (en) * | 2010-02-24 | 2011-08-31 | University College Cork-National University of Ireland, Cork | Modified graphene structure and method of manufacture thereof |
| CN102530910A (en) * | 2010-12-22 | 2012-07-04 | 海洋王照明科技股份有限公司 | Method for preparing fluorinated graphene |
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