CN104233454A - Method for effectively synthesizing monocrystal hexagonal boron nitride structure by substitution reaction - Google Patents

Method for effectively synthesizing monocrystal hexagonal boron nitride structure by substitution reaction Download PDF

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Publication number
CN104233454A
CN104233454A CN201410269988.1A CN201410269988A CN104233454A CN 104233454 A CN104233454 A CN 104233454A CN 201410269988 A CN201410269988 A CN 201410269988A CN 104233454 A CN104233454 A CN 104233454A
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substitution reaction
boron nitride
crucible
oxide powder
reaction method
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刘飞
许宁生
邓少芝
陈军
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Sun Yat Sen University
National Sun Yat Sen University
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National Sun Yat Sen University
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Abstract

The invention discloses a method for effectively synthesizing a monocrystal hexagonal boron nitride structure by a substitution reaction. The method adopts boron oxide powder and a carbon sourced material as reacting raw materials, and comprises the step of carrying out the substitution reaction for 2-8 hours at 1100-1800 DEG C in a high-temperature electric furnace by using N2 and/or NH3 as a reacting carrier gas to synthesize the monocrystal hexagonal boron nitride laminated structure. The boron nitride structure prepared by the method can be of a laminated structure, a banded structure, a tubular structure, a tower structure or a spherical structure and the like. The preparation method is simple, and has the advantages of high productivity (more than 20 percent), high yield, and high reacting speed, and the product has the advantages of high purity, good monocrystal property, excellent mechanical performance and the like.

Description

A kind of substitution reaction method of efficient synthetic single crystal hexagonal boron nitride structure
Technical field
The present invention relates to a kind of method of synthesizing boron nitride laminated structure, particularly a kind of method utilizing high temperature substitution reaction technique to high-efficiency to prepare monocrystalline hexagonal boron nitride structure.
Background technology
Since the scientist An Deliehaimu of Univ Manchester UK in 2010 and Constantine Nuo Woxiaoluofu relies on their systematic study on Graphene to obtain Nobel Prize in physics, receive increasing concern with Graphene with the New Two Dimensional nanostructure of representative.And among the two-dimensional nanostructure that these are novel, boron nitride two-dimensional layered structure has high Young's modulus (36.5GPa), high-melting-point (3200K), high heat conductance (20Wcm -1k -1), low density (2.1g/cm 3) and the advantage such as very large direct band gap (5.5eV), and have the structure quite similar with Graphene, so become the focus that domestic and international investigators pay close attention to gradually.Boron nitride structure owing to having unique physics and chemistry characteristic, so all have great application prospect in ultraviolet laser, advanced ceramics matrix material, solid lubricant, bio-sensing and piezoelectricity field.
In recent years, a lot of research group has been had to utilize diverse ways to attempt synthesis boron nitride layer shape structure.As: Osterwalder group (the J.Osterwalder et al. of Switzerland, Science303 (2004) 217) in the system of ultrahigh vacuum(HHV), at the temperature of 1070K, utilize borazine gas as raw material, clean Rh (111) substrate has prepared BN laminated structure first; People (the C.Y.Zhi et al. such as the Zhi Chunyi of Japan, Adv.Mater.21 (2009) 2889) using boron oxide powder as source material, use DMF (N, dinethylformamide) as the solvent disperseing boron nitride powder, utilize the ultrasonic apparatus ultrasonic disperse of super high power within 10 hours, to obtain few layer of a small amount of boron nitride laminated structure; The people such as the Shi of Nanyang Technological University (Y.M.Shi et al., Nano Lett.10 (2010) 4134) utilize borazine gas and nitrogen as reactant gas source, adopt chemical Vapor deposition process, the Si substrate covering Ni catalyst film has synthesized boron nitride laminated structure; The Cui get Liang group (D.L.Cui et al., J.Mater.Chem.A1 (2013) 5105) of Shandong Province of China university utilizes NaBH 4, NaN 3, NH 4cl and sublimed sulphur are source material, utilize the laminated structure etc. of water heat transfer boron nitride.
But sum up preparation method recited above, we find that most preparation methods always exists following point more or less: the productive rate as boron nitride laminated structure is low, crystalline quality is poor and source material is expensive or toxicity is larger.And these problems cause a lot of inconvenience in the industrial production of reality and application, which prevent fast development and the use of boron nitride laminated structure.Therefore find a kind of can efficiently, the green preparation process of low cost and synthetic single crystal boron nitride laminated structure just becomes very necessary.
Summary of the invention
The object of the present invention is to provide a kind of novel method adopting simple high temperature substitution reaction to carry out high yield to prepare mono-crystal nitride boron laminated structure.
The present invention solves the problem of the prior art by the following technical solutions, a kind of substitution reaction method of efficient synthetic single crystal hexagonal boron nitride structure, using boron oxide powder and carbon source material as reaction raw materials, carries out high temperature substitution reaction, comprises the following steps:
(a) raw-material placement: the bottom first a certain amount of boron oxide powder being placed on crucible, more in proportion by appropriate carbon source material uniform fold on powder upper strata, then will be equipped with raw-material crucible be transmitted into reaction electric furnace in;
(b) substitution reaction: first reaction electric furnace vacuum tightness is evacuated to 5-20Pa, then passes into N 2and/or NH 3mixed gas, make to maintain certain air pressure in reaction electric furnace; Again at N 2and/or NH 3atmosphere in, starting material are rapidly heated to growth temperature, and insulation growth for some time, namely by this substitution reaction synthetic single crystal boron nitride structure.
Above-mentioned carbon source material comprises: powdered graphite, activated carbon powder, amorphous carbon dust, high reductibility carbon dust, carbon black, single armed, both arms or multi-arm carbon nano-tube.
The mass ratio B of above-mentioned boron oxide powder and carbon source material 2o 3: C is 3:1-10:1.
Above-mentioned crucible is high-melting-point crucible, comprises plumbago crucible, BN crucible or corundum crucible.
Above-mentioned reaction electric furnace comprises thermal evaporation stove, tube furnace, retort furnace, induction heat stove, box-type furnace, electron beam process furnace, microwave oven or LASER HEATING stove.
Above-mentioned N 2and NH 3the flow proportional of mixed gas is 100:0-100:20.
The air pressure reacting reactive system in electric furnace in above-mentioned steps b is 0.1-1 normal atmosphere.
The temperature being incubated growth in above-mentioned steps b is 1100-1800 DEG C, and temperature rise rate is 40-200 DEG C/min.
Being incubated growth time in above-mentioned steps b is 2-8 hour.
Described boron nitride structure, according to regulation and control growthing process parameter, can obtain the different morphologies such as laminated structure, zonal structure, tubular structure, tower structure and ball-like structure.
Adopt above-mentioned preparation method, according to adjusting process parameter, utilize different carbon sources, effectively can realize the high yield preparation of mono-crystal nitride boron laminated structure.
Compared with prior art, the invention has the beneficial effects as follows:
The output capacity of the boron nitride structure prepared by the inventive method can reach 15%-25%, and product has even, the monocrystalline good and advantage that chemical composition is single of pattern, the carbon source material simultaneously used and boron oxide powder have low cost, free of contamination advantage, and substitution reaction can once complete, so also have simple and advantage efficiently.In sum, the present invention is very suitable for large-scale production and the application of monocrystalline hexagonal boron nitride structure for the preparation of the substitution reaction method of boron nitride structure.
Accompanying drawing explanation
Fig. 1 is the photo of the monocrystalline BN laminated structure utilizing substitution reaction method of the present invention to synthesize at different batches;
Fig. 2 A uses Graphite Powder 99 and boron oxide powder as starting material in the present invention, the low power SEM figure of synthesized boron nitride monocrystal laminated structure;
Fig. 2 B uses Graphite Powder 99 and boron oxide powder as starting material in the present invention, the high power SEM figure of synthesized boron nitride monocrystal laminated structure;
Fig. 3 A uses multi-arm carbon nano-tube powder and boron oxide powder as starting material in the present invention, the low power SEM figure of synthesized boron nitride monocrystal laminated structure;
Fig. 3 B uses multi-arm carbon nano-tube powder and boron oxide powder as starting material in the present invention, the high power SEM figure of synthesized boron nitride monocrystal laminated structure;
Fig. 4 A uses activated carbon powder and boron oxide powder as starting material in the present invention, the low power SEM figure of synthesized boron nitride monocrystal laminated structure;
Fig. 4 B uses activated carbon powder and boron oxide powder as starting material in the present invention, the high power SEM figure of synthesized boron nitride monocrystal laminated structure;
Fig. 5 is the XRD figure of the mono-crystal nitride boron lamella utilized in the present invention prepared by three kinds of different carbon source;
Fig. 6 is the Raman figure of the mono-crystal nitride boron lamella utilized in the present invention prepared by three kinds of different carbon source;
Fig. 7 A is the low power TEM figure of mono-crystal nitride boron laminated structure prepared in the present invention;
Fig. 7 B is the high power TEM figure of mono-crystal nitride boron laminated structure prepared in the present invention;
Fig. 8 is the EELS spectrum of the mono-crystal nitride boron laminated structure prepared by substitution reaction method of the present invention;
Fig. 9 is the N of different ratios 2and NH 3the XRD figure of BN laminated structure prepared under mixed-gas atmosphere;
Figure 10 A is N in reactant gases 2and NH 3the high power SEM image of the BN sample prepared when being 2SLM:0.1SLM of ratio;
Figure 10 B is N in reactant gases 2and NH 3the low power SEM image of the BN sample prepared when being 2SLM:0.1SLM of ratio;
Figure 10 C is N in reactant gases 2and NH 3the high power SEM image of the BN sample prepared when being 4SLM:0.1SLM of ratio;
Figure 10 D is N in reactant gases 2and NH 3the low power SEM image of the BN sample prepared when being 4SLM:0.1SLM of ratio;
Figure 10 E is N in reactant gases 2and NH 3the high power SEM image of the BN sample prepared when being 2SLM:0SLM of ratio;
Figure 10 F is N in reactant gases 2and NH 3the low power SEM image of the BN sample prepared when being 2SLM:0SLM of ratio;
Figure 11 A is the low power SEM image utilizing carbon black powder and the boron oxide powder BN ball-like structure prepared by starting material;
Figure 11 B is the high power SEM image utilizing carbon black powder and the boron oxide powder BN ball-like structure prepared by starting material;
Figure 12 is the SEM image utilizing multi-arm carbon pipe powder and the boron oxide powder BN tower structure prepared by starting material;
Figure 13 is the SEM image utilizing multi-arm carbon pipe powder and the boron oxide powder BN tubular structure prepared by starting material;
Figure 14 A is the SEM image utilizing multi-arm carbon pipe powder and the boron oxide powder BN zonal structure prepared by starting material;
Figure 14 B is the TEM image utilizing multi-arm carbon pipe powder and the boron oxide powder BN zonal structure prepared by starting material.
Embodiment
The starting material used in the present invention are boron oxide powder and different carbon sources.Concrete synthesis technique is high temperature substitution reaction.
The carbon source that growing single-crystal boron nitride laminated structure uses is powdered graphite, activated carbon powder, amorphous carbon dust, high reductibility carbon dust, single armed, both arms or multi-arm carbon nano-tube and carbon black etc., the crucible of carrying raw material powder can be the high-melting-point crucibles such as plumbago crucible, BN crucible and corundum crucible, and the electric furnace occurred needed for substitution reaction comprises thermal evaporation stove, tube furnace, retort furnace, induction heat stove, box-type furnace, electron beam process furnace, microwave oven or LASER HEATING stove etc.
Concrete grammar is: the upper strata first carbon source being covered in equably boron oxide powder, puts into reaction electric furnace; It is 5-20Pa that reaction electric furnace is evacuated to vacuum tightness, then passes into N 2and/or NH 3mixed gas make reaction pressure maintain between 0.1-1 normal atmosphere; With the heat-up rate of 40-200 DEG C/min, starting material are warming up to 1100-1800 DEG C again, insulation growth 2-8h.
Embodiment
The present invention is explained below in conjunction with specific embodiment, but the scope that these embodiments do not limit the present invention in any way.
Embodiment one: use Graphite Powder 99 and boron oxide powder to prepare the method for monocrystalline BN laminated structure
Covered by Graphite Powder 99 above boron oxide powder, the ratio of Graphite Powder 99 and boron oxide powder is 3:1 (weight), and system vacuum is evacuated to 15Pa, then passes into N 2gas, the system air pressure of making maintains 1 normal atmosphere; Be rapidly heated by starting material to 1400 DEG C, temperature rise rate is 50 DEG C/min again, and insulation growth 6h, namely by the high-purity boron nitride structure of efficient substitution reaction synthesis white, as shown in Figure 1.The BN single-chip Rotating fields prepared in this way, the SEM image of sample as shown in Figure 2, from figure we can observe prepared by the diameter of boron nitride monocrystal laminated structure that grows be 3-5 μm, thickness is about 20-40nm, its pattern is single simultaneously, is evenly distributed.Fig. 5 is its XRD figure, Fig. 6 is its Raman spectrogram, Fig. 7 is that its TEM schemes and Fig. 8 is its EELS collection of illustrative plates, and can prove that prepared laminated structure is monocrystalline hexagonal AlN structure, the average number of plies of laminated structure is approximately 60 simultaneously.
Embodiment two: use multi-arm carbon pipe powder and boron oxide powder to prepare the method for monocrystalline BN laminated structure
By multi-arm carbon pipe powder uniform fold on the top layer of boron oxide powder, multi-arm carbon pipe powder and boron oxide powder are by weight being 6:1 configuration.Then the N that flow proportional is 2SLM:0.1SLM is passed into 2and NH 3gas mixture, make the air pressure of reactive system in reaction electric furnace maintain between 0.5 normal atmosphere; Be rapidly heated by starting material to 1500 DEG C, temperature rise rate is 60 DEG C/min, and insulation growth 4h, can synthesize white high-purity boron nitride structure.The BN single-chip Rotating fields prepared in this way, the SEM image of sample as shown in Figure 3, from figure we can observe prepared by the diameter of boron nitride monocrystal laminated structure that grows be 1-2 μm, thickness is about 10-30nm.Their patterns are single equally, distribute also very even.Fig. 5 is the XRD figure of obtained boron nitride monocrystal laminated structure, Fig. 6 is Raman spectrum, Fig. 7 is that its TEM schemes and Fig. 8 is its EELS collection of illustrative plates, above-mentioned pattern proves that prepared laminated structure is monocrystalline hexagonal AlN structure equally, and the average number of plies of laminated structure is approximately 50 simultaneously.
Embodiment three: use activated carbon powder and boron oxide powder to prepare the method for monocrystalline BN laminated structure
By the top of activated carbon powder uniform fold boron oxide powder (weight ratio is 4:1), activated carbon powder and boron oxide powder are by weight being 4:1 configuration.Then the N that flow proportional is 4SLM:0.1SLM is passed into 2and NH 3gas mixture, make the air pressure of reactive system in reaction electric furnace maintain between 0.8 normal atmosphere; Be rapidly heated by starting material to 1600 DEG C, temperature rise rate is 80 DEG C/min, and insulation growth 8h, just can obtain white high-purity boron nitride structure.The BN single-chip Rotating fields prepared in this way, the SEM image of sample as shown in Figure 4, from figure we can observe prepared by the diameter of boron nitride monocrystal laminated structure that grows be 2-6 μm, thickness is about 20-70nm.Their pattern is single, is evenly distributed.Fig. 5 is its XRD figure, Fig. 6 is Raman spectrogram, Fig. 7 is that TEM schemes, and Fig. 8 is EELS figure.They can both prove that prepared laminated structure is monocrystalline hexagonal AlN structure, and the average number of plies of laminated structure is approximately 70 simultaneously.
These results of study show: the change of carbon source material can't affect the pattern of high purity BN laminated structure, component and monocrystalline.Therefore can obtain conclusion, high temperature substitution technique is prepared BN single-chip Rotating fields and is had good universality.
Embodiment four: prepare BN laminated structure under different carrier gas ratio
Constant at maintenance growth air pressure, using multi-arm carbon pipe and boron oxide powder (weight ratio is for 4:1) as starting material, in starting material, the ratio of multi-arm carbon pipe and boron oxide powder is 4:1 (weight).Change the ratio of growth gasses, prepare boron nitride laminated structure.Fig. 9 gives the XRD figure spectrum of the BN sample synthesized under different growth gasses ratio.Can find from figure, as N in mixed gas 2and NH 3ratio when changing to 4SLM:0.1SLM to 2SLM:0.1SLM from 2SLM:0, crystal property and the structure of BN sample do not change, and this shows in the growth gasses proportional range that provides in the present invention, i.e. N 2and NH 3the airshed of mixed gas, can synthetic single crystal hexagonal boron nitride laminated structure in the scope of 100:0-100:5.
The SEM of the BN laminated structure simultaneously prepared under gas with various ratio sees Figure 10.Figure 10 (A, B) give N 2and NH 3the SEM figure of ratio BN sample when being 2SLM:0.1SLM.Can find from figure, now BN lamella is uniform triangular morphology, and its length of side mean value is 1 μm, thickness average out to 50nm.And Figure 10 (C, D) then gives N 2/ NH 3the SEM figure of the BN sample of ratio when being 4SLM:0.1SLM.We find to work as NH 3when ratio reduces, BN pattern is gradually varied to hexagon, and mean diameter is about 1.2 μm, and thickness is about 50nm.When further by N 2/ NH 3ratio when being reduced to as 2SLM:0SLM, the pattern of BN sample there is no and changes, and just mean diameter slightly increases, and be about 1.3 μm, but chemical composition and crystallinity does not all change, still remains six side's single crystal structure.
Embodiment five: utilize carbon black powders and boron oxide powder to prepare the method for BN ball-like structure
By weight the ratio being 2:1, carbon black powders fully mixed with boron oxide powder, system vacuum is evacuated to 10Pa, then passes into the N of 3SLM 2gas, the system air pressure of making maintains 0.8 normal atmosphere; Be rapidly heated by starting material to 1200 DEG C, temperature rise rate is 60 DEG C/min, and insulation growth 4h, namely by high temperature substitution reaction synthesis boron nitride ball-like structure, as shown in Figure 11 A and 11B.From figure we can observe prepared by the diameter of boron nitride ball-like structure that grows be 100-400nm, its pattern is single simultaneously, is evenly distributed.
Embodiment six: utilize multi-arm carbon pipe powder and boron oxide powder to prepare the method for BN tower structure
By multi-arm carbon pipe powder uniform fold above boron oxide powder, wherein the boron oxide powder of multi-arm carbon pipe powder is by weight being 5:1 configuration.Then the N that flow proportional is 2SLM:0.4SLM is passed into 2and NH 3gas mixture, the system air pressure of making maintains 0.9 normal atmosphere; Be rapidly heated by starting material to 1400 DEG C, temperature rise rate is 50 DEG C/min, and insulation growth 4h, namely by high temperature substitution reaction synthesis boron nitride tower structure, as shown in figure 12.From figure we can observe prepared by the diameter of boron nitride tower structure that grows be 200-500nm, mean length is 5 μm, and it is evenly distributed, and has unified multilayer side structure.
Embodiment seven: utilize multi-arm carbon pipe powder and boron oxide powder to prepare the method for BN tubular structure
By multi-arm carbon pipe powder uniform fold above boron oxide powder, multi-arm carbon pipe powder and boron oxide powder weight ratio are 8:1.Then N is passed into 2and NH 3gas mixture, N 2and NH 3flow proportional be 2SLM:0.05SLM.Make system air pressure maintain 1 normal atmosphere simultaneously; Be rapidly heated by starting material to 1100 DEG C, temperature rise rate is 40 DEG C/min, and insulation growth 2h, namely by high temperature substitution reaction synthesis boron nitride tubular structure, as shown in figure 13.From figure we can observe prepared by the diameter of boron nitride tubular structure that grows be 10-30nm, mean length is 3 μm, has uniform nano tube structure.
Embodiment eight: utilize multi-arm carbon pipe powder and boron oxide powder to prepare the method for BN zonal structure
Multi-arm carbon pipe powder and boron oxide powder are mixed by weight the ratio uniform being 7:1, then passes into the N that flow proportional is 2SLM:0.1SLM 2and NH 3gas mixture, the system air pressure of making maintains 1 normal atmosphere; Be rapidly heated by starting material to 1300 DEG C, temperature rise rate is 50 DEG C/min, and insulation growth 4h, namely by high temperature substitution reaction synthesis boron nitride zonal structure.Figure 14 A and 14B sets forth SEM and the TEM figure of boron nitride zonal structure.From figure we can observe prepared by the width of boron nitride zonal structure that grows be 20-50nm, mean length is 4 μm, has uniform two-dimentional zonal structure.
Pole plate, hereto, mair motor drives chain guide, and has completed by the wire wheel brush of high speed rotating and take on the ear of pole plate, and the unnecessary lead plaster of circumferential side frame, zone of oxidation and the braking of burr brush are done, and make it to become light neatly.
The present invention is not limited to above-mentioned embodiment, if do not depart from the spirit and scope of the present invention to various change of the present invention or distortion, if these are changed and distortion belongs within claim of the present invention and equivalent technologies scope, then the present invention is also intended to comprise these changes and distortion.

Claims (10)

1. a substitution reaction method for efficient synthetic single crystal hexagonal boron nitride structure, is characterized in that, using boron oxide powder and carbon source material as reaction raw materials, carries out high temperature substitution reaction, comprises the following steps:
(a) raw-material placement: the bottom first a certain amount of boron oxide powder being placed on crucible, more in proportion by appropriate carbon source material uniform fold on powder upper strata, then will be equipped with raw-material crucible be transmitted into reaction electric furnace in;
(b) substitution reaction: first reaction electric furnace vacuum tightness is evacuated to 5-20Pa, then passes into N 2and/or NH 3mixed gas, make to maintain certain air pressure in reaction electric furnace; Again at N 2and/or NH 3atmosphere in, starting material are rapidly heated to growth temperature, and insulation growth for some time, namely by this substitution reaction synthetic single crystal boron nitride structure.
2. substitution reaction method according to claim 1, is characterized in that: described carbon source material comprises: powdered graphite, activated carbon powder, amorphous carbon dust, high reductibility carbon dust, carbon black, single armed, both arms or multi-arm carbon nano-tube.
3. substitution reaction method according to claim 1, is characterized in that: the mass ratio B of described boron oxide powder and carbon source material 2o 3: C is 3:1-10:1.
4. substitution reaction method according to claim 1, is characterized in that: described crucible is high-melting-point crucible, comprises plumbago crucible, BN crucible or corundum crucible.
5. substitution reaction method according to claim 1, is characterized in that: described reaction electric furnace comprises thermal evaporation stove, tube furnace, retort furnace, induction heat stove, box-type furnace, electron beam process furnace, microwave oven or LASER HEATING stove.
6. substitution reaction method according to claim 1, is characterized in that: described N 2and NH 3the flow proportional of mixed gas is 100:0-100:20.
7. substitution reaction method according to claim 1, is characterized in that: the air pressure reacting reactive system in electric furnace in described step b is 0.1-1 normal atmosphere.
8. substitution reaction method according to claim 1, is characterized in that: the temperature being incubated growth in described step b is 1100-1800 DEG C, and temperature rise rate is 40-200 DEG C/min.
9. the substitution reaction method according to claim arbitrary in claim 1 ~ 8, is characterized in that: being incubated growth time in described step b is 2-8 hour.
10. the monocrystalline hexagonal boron nitride structure that substitution reaction method according to claim 9 obtains is laminated structure, zonal structure, tubular structure, tower structure or ball-like structure.
CN201410269988.1A 2014-06-17 2014-06-17 Method for effectively synthesizing monocrystal hexagonal boron nitride structure by substitution reaction Pending CN104233454A (en)

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CN114478020A (en) * 2020-10-23 2022-05-13 中国科学院理化技术研究所 Large-size high-crystallinity h-BN ceramic material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN109518278A (en) * 2018-11-12 2019-03-26 厦门大学 A kind of method of richness nitrogen atmosphere enhancing boron nitride pellicle p-type electric-conducting doping
CN109518278B (en) * 2018-11-12 2020-12-08 厦门大学 Method for enhancing p-type conductive doping of boron nitride film by nitrogen-rich atmosphere
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CN110067027B (en) * 2019-04-19 2021-05-18 东南大学 Method for improving yield of bulk hexagonal phase boron nitride single crystal
CN114478020A (en) * 2020-10-23 2022-05-13 中国科学院理化技术研究所 Large-size high-crystallinity h-BN ceramic material and preparation method thereof
CN114478020B (en) * 2020-10-23 2023-04-28 中国科学院理化技术研究所 Large-size high-crystallinity h-BN ceramic material and preparation method thereof

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Application publication date: 20141224