CN104532209A - Method for preparing wafer-grade large-size hexagonal boron nitride on substrate - Google Patents
Method for preparing wafer-grade large-size hexagonal boron nitride on substrate Download PDFInfo
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- CN104532209A CN104532209A CN201510039073.6A CN201510039073A CN104532209A CN 104532209 A CN104532209 A CN 104532209A CN 201510039073 A CN201510039073 A CN 201510039073A CN 104532209 A CN104532209 A CN 104532209A
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Abstract
The invention relates to hexagonal boron nitride, particularly a method for preparing wafer-grade large-size hexagonal boron nitride on a substrate. The method comprises the following steps: growing a hexagonal boron nitride film on Cu foil in a controllable way; after Borazane-carrying gas leaves the quartz tube, bending the Cu foil substrate into a semicircular column, putting in a quartz boat, pushing into a heating region, vacuumizing, heating, introducing H2 when the temperature reaches the set value to perform surface oxide removal treatment, further raising the growth temperature of the third region, and heating a precursor of the first region; when the set values of the first region and third region are simultaneously reached, introducing H2 and Borazane gas generated by Ar delivery from the quartz tube into a reaction chamber to react until the Cu foil is completely covered; after the reaction finishes, taking out the Cu foil, thereby obtaining the large-area hexagonal boron nitride film on the Cu foil; and applying a PMMA (polymethyl methacrylate) layer by spin coating, dissolving away the Cu substrate, transferring the PMMA/hexagonal boron nitride film onto the substrate, and removing the PMMA layer on the sample surface.
Description
Technical field
The present invention relates to hexagonal boron nitride, particularly relate to a kind of method preparing wafer scale large size hexagonal boron nitride in substrate.
Background technology
Due to sapphire application widely, such as LED, solar cell, metal-oxide-semiconductor, silicon single crystal wafer, diode etc.If directly stablely on a sapphire substrate can shift upper h-BN, this will more be conducive to the performance test of h-BN, and is prepared into new opto-electronic device.
Because h-BN has extraordinary performance, such as there are high thermal conductance, high mechanical strength, high chemical stability, high resistance resistive etc., h-BN is made to have boundless application prospect, it can be used in heat interfacial material, as LED, LCD, TV, mobile phone, computer, telecommunication apparatus etc., also can as the substrate of coating and Graphene.Can be synthesized h-BN nano thin-film by different modes now, such as: micromechanics stripping method, solution method, MOCVD, APCVD, LPCVD etc.At present in the process of application CVD method synthesis h-BN, be all use different types of metal as substrate.
In New Generation Optical electrical part and microprocessor applications, the demand for large-area high-quality hexagonal boron nitride is more strong.Therefore, if the growth of boron nitride can be controlled very well, obtain the boron nitride of big area number of plies controllable precise, tool is of great significance.
Summary of the invention
Object of the present invention is intended to the problems such as little for existing hexagonal boron nitride area, fraction of coverage is not high, homogeneity is bad, provides a kind of method preparing wafer scale large size hexagonal boron nitride in substrate of big area, high quality, thickness controllable precise.
The present invention includes following steps:
1) controllable growth hexagonal boron nitride thin layer on Cu paper tinsel, concrete grammar is as follows: by three-temperature-zone LPCVD system, with Borazane powder as reaction source, first, Cu paper tinsel is put into quartz boat, pushes CVD reaction chamber heating warm area, Borazane powder is placed in built-in silica tube, vacuumize in chamber, then use tube furnace to heat quartz reaction chamber.When three district's reaction chamber temperatures reach set(ting)value (800 ~ 1000 DEG C), first pass into H2, carry out the process of surperficial deoxidation compound, continue the growth temperature in rising three district, and district's precursor is heated simultaneously, and when reaching set(ting)value one district temperature (60 ~ 80 DEG C) and three district's temperature (1000 ~ 1050 DEG C), from silica tube, pass into H simultaneously
2enter reaction chamber with the Borazane gas of Ar conveying generation to react, after question response terminates, sample is pulled out heating zone, pass into H simultaneously
2be used as shielding gas with Ar, finally in time dropping to room temperature, take out sample; Through carrying out opticmicroscope and SEM test to its surface, the hexagonal boron nitride thin layer of growth on Cu paper tinsel can be observed;
2) after the gas carrying Borazane leaves silica tube, Cu paper tinsel substrate is bent to the semi-cylindrical of axle centered by silica tube and folding inserts quartz boat, push CVD reaction chamber heating warm area, chamber internal gas pressure is evacuated to 10
-3about torr, then heats quartz reaction chamber with tube furnace, when temperature reaches set(ting)value, first passes into H
2carry out the process of surperficial deoxidation compound, continue the growth temperature in rising three district afterwards, and district's precursor is heated simultaneously, when reaching set(ting)value one district temperature (60 ~ 80 DEG C) and three district's temperature (1000 ~ 1050 DEG C), from silica tube, pass into H simultaneously
2enter reaction chamber with the Borazane gas of Ar conveying generation to react, until Cu paper tinsel is completely covered, reaction terminates rear taking-up Cu paper tinsel, carries out opticmicroscope and SEM test, can observe the big area hexagonal boron nitride thin layer of growth on Cu paper tinsel to Cu paper tinsel surface;
3) spin coating pmma layer on the Cu paper tinsel having hexagonal boron nitride thin layer is being grown, then ammonium persulphate is utilized to dissolve Cu substrate, recycle means of transferring by pmma/ hexagonal boron nitride film transfer on substrate, finally put into acetone soln to soak, remove the pmma layer of sample surfaces, namely complete and prepare wafer scale large size hexagonal boron nitride in substrate.
In step 1) in, describedly to vacuumize in chamber, can utilize mechanical pump and molecular pump that chamber internal gas pressure is evacuated to 10
-3about torr; The time of described surperficial deoxidation compound process can be 10 ~ 30min; Describedly from silica tube, pass into H
24 ~ 8sccm and 10 ~ 20sccm is respectively with the amount of Ar; Describedly pass into H simultaneously
28 ~ 15sccm and 10 ~ 20sccm is respectively with the amount of Ar.
In step 2) in, describedly to vacuumize in chamber, can utilize mechanical pump and molecular pump that chamber internal gas pressure is evacuated to 10
-3about torr; The time of described surperficial deoxidation compound process can be 10 ~ 30min; H is passed into from silica tube
24 ~ 8sccm and 10 ~ 20sccm is respectively with the amount of Ar; The diameter of described big area hexagonal boron nitride thin layer can be 2 ~ 4 inches.
In step 3) in, described means of transferring can adopt grafter, especially large-sized grafter; The diameter of described substrate can be 2 ~ 4 inches; Described substrate can adopt Sapphire Substrate, Si sheet, silica glass, metal, plastic flexible films etc., preferred Sapphire Substrate.
The present invention is in order to improve the quality of the h-BN of acquisition better, sapphire application in optoelectronic devices can be expanded further simultaneously, propose growth and transferring plates level large size hexagonal boron nitride, can significantly improve h-BN quality and output, thus obtain high-quality opto-electronic device.From application point, this material applied by the opto-electronic device such as LED, solar cell, be expected to improve its light output, efficiency of light absorption, and then improve its external quantum efficiency, life-span and the job stability of LED can also be extended.
The present invention adopts at the built-in little silica tube of CVD large silica tube heating chamber, utilize the principle of the spherical diffusion of gas in vacuum, in conjunction with symmetrical semi-circular post Copper Foil substrate, realize the uniform h-BN atomic layer level thin film of little raw material growing large-area, utilize quartzy magnetic rod to reach the object of rapid temperature rise and drop simultaneously, in temperature-fall period, keep surfacing to make hexagonal boron nitride.Design a whole set of large-sized grafter instrument, there is function that solution leaks filter, flat support respectively, realize stable entirely atom film transfer.By the hBN of the stable transfer large-area ultrathin of PMMA transfer method in any target substrate.The hexagonal boron nitride of the present invention LPCVD method growing large-area on Copper Foil and successfully transferring in target substrate, this kind of method makes it possible to achieve the large output of few raw material, for a large amount of production provides possibility.
Accompanying drawing explanation
Fig. 1 is the three-temperature-zone LPCVD system schematic of the embodiment of the present invention.
Fig. 2 is the SEM figure of the hexagonal boron nitride grown on Cu paper tinsel at 1050 DEG C.
Fig. 3 is the SEM figure that growth time is respectively the Graphene that 5min, 10min, 30min, 40min grow on Cu paper tinsel.
Fig. 4 is that hexagonal boron nitride transfers to Raman spectrum on silicon chip.
Fig. 5 is that hexagonal boron nitride transfers to XPS spectrum on silicon chip (B1s).
Fig. 6 is that hexagonal boron nitride transfers to XPS spectrum on silicon chip (N1s).
Fig. 7 is the SEM figure that hexagonal boron nitride successfully transfers on sapphire.
Embodiment
Embodiment one:
First, controllable growth hexagonal boron nitride on Cu paper tinsel.
1) be placed in elongated silica tube with quartz boat dress 0.5mg Borazane powder, put into three-temperature-zone CVD device, as shown in Figure 1.Adjustment position, make Borazane powder in the mid-way of the first warm area, by elongated little silica tube access ventage, again cleaned Cu paper tinsel is put into the three-temperature-zone of CVD device, and ensureing in the mid-way of three-temperature-zone, the direction along air-flow is Borazane powder, Cu paper tinsel successively.Vacuum cavity is used cushion rubber flange seal, the intensification parameter reserved in advance and ventilation parameters are inputted computer, for ready to three warm areas heating of CVD below.Start to vacuumize cavity, first adopt mechanical oil pump, reach 2 × 10 to vacuum tightness
-2during Torr, open molecular pump, to low vacuum in 9 × 10
-3start during Torr to heat according to preset parameter heating warm area.When three-temperature-zone substrate temperature reaches 800 DEG C, pass into the H that 12sccm air pressure is 30psi
2, and 20sccm air pressure is the Ar of 30psi, venting process continues 30min, and this venting process can clean oxide compound and the impurity on Cu surface.According to the parameter of temperature program setting, after ventilation 30min, stop passing into gas, three district's reaction chamber temperatures continue to increase, and when Dang Sanqu reaches 1050 DEG C, the temperature of a district Borazane just reaches design temperature 70 DEG C, passes into H immediately
2with the mixture of Ar gas as carrier gas, gas flow is respectively 8sccm/15sccm, air pressure is 30psi, now process of growth starts, the Borazane powder in one district produces Borazane gas at the temperature of 70 DEG C, under the effect of carrier gas, Borazane gas is transported to high temperature reaction zone, part Borazane gas becomes h-BN nano thin-film at Cu paper tinsel surface deposition nucleating growth.
2) PMMA transfer step:
Prepare ammonium persulfate solution, 6g ammonium persulphate ((NH
4)
2s
2o
8)+210ML (H
2o). after sample is cut out, be placed on little slide, seal by adhesive tape around sample, enter the sample back side to prevent PMMA.By sol evenning machine PMMA uniform application at sample surfaces.To treat in air after seasoning 30min, to be placed on warm table 100 DEG C, 20min (below the upper clean slide glass of pad), after cooling, sample is torn it down from slide, part sample edge not being coated PMMA is cut., float in the ammonium persulfate solution that the first step configures sample P MMA layer upward, the cleaning sample back side.The hexagonal boron nitride at the Cu dissolved and the back side is rinsed well, prevents the hexagonal boron nitride at the back side from affecting front.Every 10min with deionized water rinsing once, front and back rinse 2 ~ 3 times, afterwards sample is floated in solution, general 3h, all melts away Cu.With slide sample is transferred in deionized water and soaks 30min, sample floats on deionized water surface.Cleaning Si sheet, is placed in the ultrasonic 30min of acetone soln Si sheet, then uses the ultrasonic 30min of dehydrated alcohol.Si sheet is salvaged, and notes making sample be carried on Si sheet mid-way during salvaging, drying moisture, preventing there is bubble because there being moisture between sample and Si sheet.Drying treatment, after cleaned sample seasoning, puts into loft drier with 150 DEG C, baking 1h.Soak 10min with acetone, removing PMMA, after changing 3 acetone solns, soaks for a long time, within one day, changes a solution, 2D-3D.Draw acetone soln with syringe when changing solution, do not allow sample be exposed in air.Rinse with dehydrated alcohol, then take out.
Embodiment two: growing large-area continuous print boron nitride
1) with in embodiment one by precursor, be placed in elongated little silica tube with quartz boat dress 1mg Borazane powder, put into three-temperature-zone CVD device, as shown in Figure 1.Adjustment position, make Borazane powder in the mid-way of the first warm area, by elongated little silica tube access ventage, get the Copper Foil cleaning of 7cm × 7cm, again cleaned Cu paper tinsel is bent the three-temperature-zone putting into CVD device, and ensureing in the mid-way of three-temperature-zone, the direction along air-flow is Borazane powder, Cu paper tinsel successively.All the other steps are identical with embodiment one, increase growth time to 40min.
2) transfer step is the same, owing to shifting the increase greatly of sample area, original instrument can not be used for stablizing transfer, after Cu paper tinsel melts away completely, with big area grafter means of transferring, sample is transferred in deionized water, then carry out 2 inches sapphire sheets to salvage, sapphire sheet is fixed on big area porous means of transferring, go again to salvage sample in deionized water, following step is with transfer process above, be so just that the continuous hexagonal boron nitride film of big area of 2 inches stablizes that to transfer to diameter be in the Sapphire Substrate of 2 inches by the diameter of growth.
The above-mentioned sample transferred on silicon chip is done Raman spectrum test, found that at 1371.6cm
-1place has the peak position of stronger hexagonal boron nitride to occur.Gone by sample more in addition to survey XPS spectrum, find that B1s peak is at 190.08ev place, N1s peak, at 397.8ev place, demonstrates the grown of high-quality hexagonal boron nitride again.The series of samples of above-mentioned growth is characterized by SEM, characterization result is as shown in Fig. 2 ~ 7, illustrate that successful growth goes out big area continuous print hexagonal boron nitride film, the diameter of hexagonal boron nitride film is 2 inches, and successfully to have transferred to diameter be on the substrate of 2 inches.
The invention provides a kind of method (described large size refer to >=2 inches) preparing wafer scale large size hexagonal boron nitride in substrate.It mainly utilizes low-pressure chemical vapor deposition method (LPCVD), at the large-sized h-BN nano thin-film of Copper Foil Grown, and stable transfers on large-size sapphire substrate, make the various characteristics of easier measure sample, to obtain photoelectron device and other large-area application.First logically regulate each parameter, finally controlledly on Cu surface can grow h-BN; Then, utilize the diffusion principle of vacuum pneumatic and half reel method of Copper Foil substrate, realize the atomic shell h-BN film obtaining overlarge area with less reaction raw materials.And design a whole set of stainless steel grafter instrument, utilize PMMA transfer method, entirely wafer scale large size h-BN film is turned and be overlying on 2 inches or more large-area Sapphire Substrate, complete Van der Waals force bonding.By this technology, the h-BN atom film of high yield, high quality, overlarge area can be obtained, apply to the industrialization wafer manufacture of opto-electronic device, obtain the new device of premium properties.
Controllable growth hexagonal boron nitride on Cu paper tinsel, needs the number of plies of control hexagonal boron nitride that can be stable, monocrystalline size and area coverage.Control respectively by change precursor temperature, growth temperature and growth time, be the object that sample reaches fast cooling by magnetic rod after the growth was completed simultaneously, thus improve the growth quality of hexagonal boron nitride.
The present invention improves growth area by regulate factors, makes to stablize to cover extensive substrate, by changing experiment condition, carries out a series of experiment.In addition, utilize mechanical pump and molecular pump that vacuum is evacuated to 9 × 10
-3below, utilizing magnetic rod, when growth completes, sample is pulled out sample, fast cooling, taking out sample until system cools to beginning to speak during room temperature, fortune can make growth hexagonal boron nitride keep surfacing in this way, obtains high-quality sample.Find the area coverage that effectively can improve hexagonal boron nitride by increasing the reaction times, until cover Cu paper tinsel substrate completely, the internal diameter of CVD equipment reaction chamber is 2 inches, by bending Copper Foil, the maximum sample that can grow 4 inches of sizes, effectively improves the output of once testing.
Hexagonal boron nitride is successfully transferred to after in Sapphire Substrate, conveniently does a series of sign, and can more effectively apply in electronic device industryization production.When large-area hexagonal boron nitride growth is after Cu paper tinsel, uses solution transfer method, hexagonal boron nitride is transferred on 2 inches sapphire substrate, utilizes large size grafter instrument, realize stable entirely atom film transfer; Pmma plays middle transition effect, and ammonium persulphate is used for dissolving Cu paper tinsel, and acetone is with removing pmma.Adopt this transfer method method, hexagonal boron nitride film can be transferred in various wafer substrates well, such as Si sheet, silica glass, metal, plastic flexible films etc.
Claims (10)
1. in substrate, prepare a method for wafer scale large size hexagonal boron nitride, it is characterized in that comprising the following steps:
1) controllable growth hexagonal boron nitride thin layer on Cu paper tinsel, concrete grammar is as follows: by three-temperature-zone LPCVD system, with Borazane powder as reaction source, first, Cu paper tinsel is put into quartz boat, pushes CVD reaction chamber heating warm area, Borazane powder is placed in built-in silica tube, vacuumize in chamber, then use tube furnace to heat quartz reaction chamber; When three district's reaction chamber temperatures reach set(ting)value 800 ~ 1000 DEG C, first pass into H
2, carry out the process of surperficial deoxidation compound, continue the growth temperature in rising three district, and district's precursor is heated simultaneously, and when reaching temperature 60 ~ 80 DEG CHe tri-district of set(ting)value one district temperature 1000 ~ 1050 DEG C, from silica tube, pass into H simultaneously
2enter reaction chamber with the Borazane gas of Ar conveying generation to react, after question response terminates, sample is pulled out heating zone, pass into H simultaneously
2be used as shielding gas with Ar, finally in time dropping to room temperature, take out sample; Through carrying out opticmicroscope and SEM test to its surface, the hexagonal boron nitride thin layer of growth on Cu paper tinsel can be observed;
2) after the gas carrying Borazane leaves silica tube, Cu paper tinsel substrate is bent to axle centered by silica tube semi-cylindrical and folding insert quartz boat, push CVD reaction chamber heating warm area, vacuumize in chamber, then with tube furnace, quartz reaction chamber is heated, when temperature reaches set(ting)value, first pass into H
2, carry out the process of surperficial deoxidation compound, continue the growth temperature in rising three district afterwards, and district's precursor is heated simultaneously, when reaching temperature 60 ~ 80 DEG CHe tri-district of set(ting)value one district temperature 1000 ~ 1050 DEG C, from silica tube, pass into H simultaneously
2enter reaction chamber with the Borazane gas of Ar conveying generation to react, until Cu paper tinsel is completely covered, reaction terminates rear taking-up Cu paper tinsel, carries out opticmicroscope and SEM test, can observe the big area hexagonal boron nitride thin layer of growth on Cu paper tinsel to Cu paper tinsel surface;
3) spin coating pmma layer on the Cu paper tinsel having hexagonal boron nitride thin layer is being grown, then ammonium persulphate is utilized to dissolve Cu substrate, recycle means of transferring by pmma/ hexagonal boron nitride film transfer on substrate, finally put into acetone soln to soak, remove the pmma layer of sample surfaces, namely complete and prepare wafer scale large size hexagonal boron nitride in substrate.
2. a kind of method preparing wafer scale large size hexagonal boron nitride in substrate as claimed in claim 1, is characterized in that in step 1) and 2) in, describedly vacuumizing in chamber, is utilize mechanical pump and molecular pump that chamber internal gas pressure is evacuated to 10
-3torr.
3. a kind of method preparing wafer scale large size hexagonal boron nitride in substrate as claimed in claim 1, is characterized in that in step 1) and 2) in, the time of described surperficial deoxidation compound process is 10 ~ 30min.
4. a kind of method preparing wafer scale large size hexagonal boron nitride in substrate as claimed in claim 1, is characterized in that in step 1) in, describedly from silica tube, pass into H
24 ~ 8sccm and 10 ~ 20sccm is respectively with the amount of Ar.
5. a kind of method preparing wafer scale large size hexagonal boron nitride in substrate as claimed in claim 1, is characterized in that in step 1) in, describedly pass into H simultaneously
28 ~ 15sccm and 10 ~ 20sccm is respectively with the amount of Ar.
6. a kind of method preparing wafer scale large size hexagonal boron nitride in substrate as claimed in claim 1, is characterized in that in step 2) in, from silica tube, pass into H
24 ~ 8sccm and 10 ~ 20sccm is respectively with the amount of Ar.
7. a kind of method preparing wafer scale large size hexagonal boron nitride in substrate as claimed in claim 1, is characterized in that in step 2) in, the diameter of described big area hexagonal boron nitride thin layer is 2 ~ 4 inches.
8. a kind of method preparing wafer scale large size hexagonal boron nitride in substrate as claimed in claim 1, is characterized in that in step 3) in, described means of transferring is grafter.
9. a kind of method preparing wafer scale large size hexagonal boron nitride in substrate as claimed in claim 1, is characterized in that in step 3) in, the diameter of described substrate is 2 ~ 4 inches.
10. a kind of method preparing wafer scale large size hexagonal boron nitride in substrate as claimed in claim 1, it is characterized in that in step 3) in, described substrate adopts Sapphire Substrate, Si sheet, silica glass, metal, plastic flexible films, preferred Sapphire Substrate.
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| CN106245001A (en) * | 2016-08-05 | 2016-12-21 | 复旦大学 | Plasma enhanced chemical vapor deposition prepares the method for hexagonal boron nitride and hybrid structure thereof |
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| CN109722650A (en) * | 2019-02-15 | 2019-05-07 | 清华-伯克利深圳学院筹备办公室 | A kind of hexagonal boron nitride material and preparation method thereof and transfer method |
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| CN105508745A (en) * | 2016-01-07 | 2016-04-20 | 湖州奥博石英科技有限公司 | Quartz tube |
| CN105908152A (en) * | 2016-04-29 | 2016-08-31 | 杭州电子科技大学 | Transfer method of hexagonal boron nitride film |
| CN105908152B (en) * | 2016-04-29 | 2018-09-25 | 杭州电子科技大学 | A kind of transfer method of hexagonal boron nitride film |
| CN106245001A (en) * | 2016-08-05 | 2016-12-21 | 复旦大学 | Plasma enhanced chemical vapor deposition prepares the method for hexagonal boron nitride and hybrid structure thereof |
| CN107753023A (en) * | 2017-10-17 | 2018-03-06 | 中钢集团武汉安全环保研究院有限公司 | A kind of method for preparing stretchable respiration monitoring control material |
| CN108559973A (en) * | 2017-12-29 | 2018-09-21 | 厦门大学 | A kind of method that two dimension hexagonal boron nitride film doping obtains p-type conductance |
| GB2573812A (en) * | 2018-05-18 | 2019-11-20 | Cambridge Entpr Ltd | Synthesis And Transfer Methods |
| CN108660441B (en) * | 2018-06-15 | 2019-09-20 | 厦门大学 | A kind of transfer method of boron nitride pellicle |
| CN108660441A (en) * | 2018-06-15 | 2018-10-16 | 厦门大学 | A kind of transfer method of boron nitride pellicle |
| CN109722650A (en) * | 2019-02-15 | 2019-05-07 | 清华-伯克利深圳学院筹备办公室 | A kind of hexagonal boron nitride material and preparation method thereof and transfer method |
| CN111575674A (en) * | 2019-02-15 | 2020-08-25 | 中国科学院物理研究所 | Hexagonal boron nitride film and preparation method thereof |
| CN109722650B (en) * | 2019-02-15 | 2021-09-28 | 清华-伯克利深圳学院筹备办公室 | Hexagonal boron nitride material and preparation method and transfer method thereof |
| CN111826712A (en) * | 2019-04-15 | 2020-10-27 | 中国科学院化学研究所 | Method for preparing wafer-level uniform hexagonal boron nitride film |
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| CN113380603A (en) * | 2021-05-18 | 2021-09-10 | 厦门大学 | High-boron-component two-dimensional III-group multi-element nitride mixed crystal and preparation method thereof |
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