CN1327046C - Monocrystalline Si3N4 nanometer belt and micro belt preparation method - Google Patents
Monocrystalline Si3N4 nanometer belt and micro belt preparation method Download PDFInfo
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- CN1327046C CN1327046C CNB2005100121882A CN200510012188A CN1327046C CN 1327046 C CN1327046 C CN 1327046C CN B2005100121882 A CNB2005100121882 A CN B2005100121882A CN 200510012188 A CN200510012188 A CN 200510012188A CN 1327046 C CN1327046 C CN 1327046C
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- si3n4
- pyrolysis
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910052581 Si3N4 Inorganic materials 0.000 title abstract 5
- 239000007787 solid Substances 0.000 claims abstract description 22
- 238000000197 pyrolysis Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 10
- 238000004132 cross linking Methods 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- 229910052802 copper Inorganic materials 0.000 claims abstract description 3
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 3
- 239000002127 nanobelt Substances 0.000 claims description 30
- 238000000498 ball milling Methods 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 14
- 238000009413 insulation Methods 0.000 claims description 14
- 229910021419 crystalline silicon Inorganic materials 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 10
- 229920001709 polysilazane Polymers 0.000 claims description 8
- 239000004677 Nylon Substances 0.000 claims description 7
- 239000002086 nanomaterial Substances 0.000 claims description 7
- 229920001778 nylon Polymers 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 229910021577 Iron(II) chloride Inorganic materials 0.000 abstract 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 abstract 1
- -1 polysiloxane Polymers 0.000 abstract 1
- 229920001296 polysiloxane Polymers 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 238000001149 thermolysis Methods 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000002041 carbon nanotube Substances 0.000 description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 description 5
- 239000003082 abrasive agent Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000005611 electricity Effects 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 238000010923 batch production Methods 0.000 description 1
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 description 1
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a preparation method for single-crystal Si3N4 nanometer strips and single-crystal Si3N4 micron strips, which belongs to the technical field of material preparation. The present invention uses an organic precursor to synthesize the single-crystal Si3N4 nanometer strips and the single-crystal Si3N4 micron strips in a thermolysis mode; the present invention comprises the steps: 1, low-temperature crosslinking solidification: initial raw material is polysiloxane and is crosslinked and solidified under the preserved temperature of 240 to 290 DEG C in nitrogen or ammonia, and semitransparent SiCN solid in an amorphous state is obtained; 2, high-energy ball milling pulverization: semitransparent SiCN solid is milled in a high-energy ball mill and simultaneously a catalyst which is any one kind of FeCl2, Al, Cu, Ni and Fe and has 1 to 5 wt% using amount is introduced in the semi-transparent SiCN solid; 3, high-temperature pyrolysis: the high-temperature pyrolysis is carried out to mixtures after the high-energy ball milling, and the temperature is preserved under the pyrolysis temperature of 1250 to 1550 DEG C. The method has the advantages of simple technique, strong maneuverability and high synthesis product purity; the present invention can prepare lower-dimensional nanometer material such as nanometer wires, nanometer belts, nanometer rods, etc. with different patterns by simply controlling a plurality of key process parameters.
Description
Technical field
The present invention relates to a kind of single crystalline Si
3N
4The preparation method of nanobelt and micro belt belongs to technical field of material.
Background technology
Nano strip material is a kind of new function material.Recently, the artificial representatives such as professor Wang Zhonglin with the georgia ,u.s.a Institute of Technology utilize the high-temp solid vapor phase process to successfully synthesize the nano strip structure of a series of broadband semiconductor systems such as zinc oxide, stannic oxide, Indium sesquioxide, Cadmium oxide and gallium oxide.These zonal structure purity height, output are big, perfect structure, surface clean, and inner zero defect, dislocation-free and fault, are the linear type lamellar structures of an ideal monocrystalline.Compare with carbon nanotube and other nanometer linear structures, nano belt is that only so far being found has controllable structure and flawless accurate one dimension zonal structure, and has structure and the physicals unique and more superior than carbon nanotube.Carbon nanotube hardness height, electroconductibility is very strong, and these characteristics make it become favorite in the nano science research of the nineties in 20th century.But CNT defective can occur when batch production.The defective electronic component of material is by electric current the time, and temperature may raise unusually.And there is not the stability problem of carbon nanotube in synthetic conductor oxidate nano belt.The purity of these ribbon construction material can be up to more than 95% simultaneously, and by contrast, the purity of carbon nanotube only reaches about 70%.These advantages of nanobelt might make it more early be put into industrial production.
Low-dimensional Si
3N
4Material has very high intensity, and is in light weight, good thermal shock and oxidation resistance, thereby have very widely at a lot of industrial circles and to use.Simultaneously, Si
3N
4Also be a kind of wide semiconductor (5.3ev) that can be with, can be with its electricity and optical property thereby can reduce it by means such as doping, thereby prepare the nano electron device that can under high temperature and high radiation environment, use.Up to the present, only there are the people such as Bando of Japan to utilize the high-temp solid vapor phase method to synthesize single crystalline Si according to the current paper report
3N
4Nanobelt and micro belt, the domestic report that yet there are no.
Summary of the invention
It is simple to the objective of the invention is to propose a kind of equipment and synthesis technique, the products collection efficiency height, the purity height, and have a good repeatability prepare single crystalline Si with the organic precursor pyrolysis
3N
4The method of nanobelt and micro belt.The nanobelt that the party's legal system is standby and the growth mechanism of micro belt and the Si that has reported
3N
4The gas-solid of nanobelt (Vapor-Solid:VS) growth mechanism difference is solid-liquid gas-solid (Solid-Liquid-Gas-Solid:LSGS) mechanism.This mechanism is very beneficial for low-dimension nano material is carried out doping treatment, thereby regulates and control its electricity and optical property, prepares the nano electron device that can use under high temperature and high radiation environment.
The single crystalline Si that the present invention proposes
3N
4The preparation method of nanobelt and micro belt is characterized in that: described method adopts organic precursor pyrolysis synthetic single crystal Si
3N
4Nanobelt and micro belt may further comprise the steps:
(1) crosslinked at low temperature solidifies: initial feed adopts polysilazane, and 240-290 ℃ of insulation carried out crosslinking curing in 0.4-4 hour in nitrogen or ammonia, obtained translucent non-crystalline state SiCN solid;
(2) high-energy ball milling is pulverized: translucent SiCN solid is packed in the nylon resin ball grinder, carry out dry ball milling and pulverize in high energy ball mill, introduce catalyzer in the time of ball milling, make that non-crystalline state SiCN powder and catalyst mix are even;
(3) high temperature pyrolysis: the mixture behind the high-energy ball milling is carried out high temperature pyrolysis, under 1250～1550 ℃ of pyrolysis temperatures, be incubated 1～8 hour, can obtain the low-dimension nano material of different-shape and chemical ingredients.Protective atmosphere is N
2Gas or ammonia.
In above-mentioned preparation method, the catalyzer of described step 2 is FeCl
2, any among Al, Cu, Ni, the Fe.
In above-mentioned preparation method, the catalyst levels of described step 2 is 1-5wt%.
The present invention has the following advantages:
1) equipment is simple, and is with low cost;
2) synthesis technique is simple, and controllability is strong, can obtain single crystalline Si by some key process parameters in the control synthesis technique
3N
4Nanobelt and micro belt, and technical process has very high repeatability;
3) synthetic product purity height, the banded structure any surface finish of being synthesized is not polluted;
4) method for preparing single crystal nano-belt and micro belt of the present invention has very high elasticity in technology, by the chemical composition at molecular level regulation and control organic precursor, can obtain the single crystal nano-belt of different chemical component;
5) the present invention's method of preparing single crystal nano-belt and micro belt is very beneficial for nano belt is carried out doping treatment, and performances such as this light for the regulation and control nano belt, electricity, heat, magnetic are very favorable, for the device of nano belt provides the foundation.
6) the prior art method for preparing nano material can only be synthesized the low-dimension nano material of single shape, and the present invention prepares the method for nano material can be prepared different-shape by the several key process parameters of simple control low-dimension nano material such as nano wire, nano belt and nanometer rod etc.
Description of drawings
Fig. 1 raw material is Polyureasilazane, and catalyst is FeCl
2, 2 hours synthetic single crystalline Si of insulation under 1350 ℃ of pyrolysis temperatures
3N
4Nanobelt SEM figure
Fig. 2 raw material is Polyureasilazane, and catalyst is Al, in 4 hours synthetic single crystalline Si of 1450 ℃ of insulations
3N
4Micro belt SEM figure
Fig. 3 raw material is Polyureasilazane and Al[OCH (CH
3)
2]
3, catalyst is FeCl
2, in 2 hours synthetic single crystalline Si with Al doping of 1450 ℃ of insulations
3N
4Nanobelt SEM figure
Fig. 4 raw material is Polysilazane, and catalyst is Fe, in 2 hours synthetic single crystalline Si of 1450 ℃ of insulations
3N
4Nanobelt SEM figure
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
Embodiment 1
Initial feed adopts liquid polysilazane (Polyureasilazane), and 260 ℃ of insulations were carried out crosslinking curing in 0.5 hour, and protective atmosphere is the N of 0.1MPa
2Gas obtains translucent non-crystalline state SiCN solid.Translucent SiCN solid packed into carry out dry ball milling in the nylon resin ball grinder pulverize in high energy ball mill, abrasive material adopts Si
3N
4Ball, Ball-milling Time are 12 hours.Introduce the FeCl of 3wt% in the time of ball milling
2Powder makes that as catalyzer non-crystalline state SiCN powder and catalyst mix are even.Get then mixture 2g behind the high-energy ball milling and pack into and carry out high temperature pyrolysis in the aluminium oxide ceramics crucible in tube furnace, Si was synthesized in insulation in 2 hours under 1350 ℃ of pyrolysis temperatures
3N
4Monocrystal nanowire.Protective atmosphere is the mobile N of 0.1MPa
2Gas, gas flow rate are 200ml/min.Synthetic Si
3N
4Single crystal nano-belt as shown in Figure 1.Single nanometer monocrystalline tape thickness and width even thickness, thickness average out to 20～40nm, width are 400～600nm, and length can reach several mm, and size is even between the nano wire, and any surface finish is not polluted.
Embodiment 2
Initial feed adopts liquid polysilazane (Polyureasilazane), and 260 ℃ of insulations were carried out crosslinking curing in 1 hour, and protective atmosphere is the N of 0.1MPa
2Gas obtains translucent non-crystalline state SiCN solid.Translucent SiCN solid packed into carry out dry ball milling in the nylon resin ball grinder pulverize in high energy ball mill, abrasive material adopts Si
3N
4Ball, Ball-milling Time are 10 hours.The Al powder of introducing 4.5wt% in the time of ball milling makes that as catalyzer non-crystalline state SiCN powder and catalyst mix are even.Get then mixture 3g behind the high-energy ball milling and pack into and carry out high temperature pyrolysis in the aluminium oxide ceramics crucible in tube furnace, Si was synthesized in insulation in 4 hours under 1450 ℃ of pyrolysis temperatures
3N
4The monocrystalline micro belt.Protective atmosphere is the mobile N of 0.1MPa
2Gas, gas flow rate are 200ml/min.Synthetic Si
3N
4The monocrystalline micro belt as shown in Figure 2.Monocrystalline micro belt width and thickness are even, and thickness is approximately 200nm, and width can reach 6 μ m, and length reaches several mm, and the micro belt any surface finish is not polluted.
Embodiment 3
Initial feed adopts two kinds of polysilazanes (Polyureasilazane and Al[OCH (CH
3)
2]
3), rear a kind of be solid state powder, at first with these two kinds of powder by weight (Polyureasilazane: Al[OCH (CH
3)
2]
3) be in nylon resin ball grinder to mix at 4: 1, carried out crosslinking curing in 0.5 hour 270 ℃ of insulations then, protective atmosphere is the N of 0.1MPa
2Gas obtains the solid particle of the amorphous Al of containing element.Solid particle packed into carry out dry ball milling in the nylon resin ball grinder pulverize in high energy ball mill, abrasive material adopts Si
3N
4Ball, Ball-milling Time are 13 hours.The Ni that introduces 3wt% in the time of ball milling makes that as catalyzer non-crystalline state powder and catalyst mix are even.Get then mixture 2g behind the high-energy ball milling and pack into and carry out high temperature pyrolysis in the aluminium oxide ceramics crucible in tube furnace, insulation was synthesized and has been had the Si that Al mixes in 2 hours under 1450 ℃ of pyrolysis temperatures
3N
4Single crystal nano-belt.Protective atmosphere is the mobile N of 0.1MPa
2Gas, gas flow rate are 200ml/min.Synthetic Si
3N
4Single crystal nano-belt as shown in Figure 3.Single monocrystalline zonal structure thickness and width are even, and thickness is approximately 80nm, and the micro belt any surface finish is not polluted.
Embodiment 4
Initial feed adopts a kind of liquid polysilazane (Polysilazane), and 280 ℃ of insulations were carried out crosslinking curing in 0.4 hour, and protective atmosphere is the N of 0.1MPa
2Gas obtains translucent non-crystalline state SiCN solid.Translucent SiCN solid packed into carry out dry ball milling in the nylon resin ball grinder pulverize in high energy ball mill, abrasive material adopts Si
3N
4Ball, Ball-milling Time are 13 hours.The Fe that introduces 1wt% in the time of ball milling makes that as catalyzer non-crystalline state SiCN powder and catalyst mix are even.Get then mixture 2g behind the high-energy ball milling and pack into and carry out high temperature pyrolysis in the aluminium oxide ceramics crucible in tube furnace, single crystalline Si was synthesized in insulation in 2 hours under 1450 ℃ of pyrolysis temperatures
3N
4Nanobelt.Protective atmosphere is the mobile N of 0.1MPa
2Gas, gas flow rate are 200ml/min.Synthetic single crystalline Si
3N
4Nanobelt as shown in Figure 4.Single nano belt thickness and width size are even, and thickness is approximately 60nm, and width is about 2um, and length reaches several mm, and the zonal structure any surface finish is not polluted.
Claims (3)
1, single crystalline Si
3N
4The preparation method of nanobelt and micro belt is characterized in that: described method adopts organic precursor pyrolysis synthetic single crystal Si
3N
4Nanobelt and micro belt may further comprise the steps:
(1) crosslinked at low temperature solidifies: initial feed adopts polysilazane, and 240-290 ℃ of insulation carried out crosslinking curing in 0.4-4 hour in nitrogen or ammonia, obtained translucent non-crystalline state SiCN solid;
(2) high-energy ball milling is pulverized: translucent SiCN solid is packed in the nylon resin ball grinder, carry out dry ball milling and pulverize in high energy ball mill, introduce catalyzer in the time of ball milling, make that non-crystalline state SiCN powder and catalyst mix are even;
(3) high temperature pyrolysis: the mixture behind the high-energy ball milling is carried out high temperature pyrolysis, be incubated 1～8 hour under 1250～1550 ℃ of pyrolysis temperatures, can obtain the low-dimension nano material of different-shape and chemical ingredients, protective atmosphere is N
2Gas or ammonia.
2, according to the described preparation method of claim 1, it is characterized in that: the catalyzer of described step 2 is FeCl
2, any among Al, Cu, Ni, the Fe.
3, according to the described preparation method of claim 1, it is characterized in that: the catalyst levels of described step 2 is 1-5wt%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100121882A CN1327046C (en) | 2005-07-15 | 2005-07-15 | Monocrystalline Si3N4 nanometer belt and micro belt preparation method |
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|---|---|---|---|
| CNB2005100121882A CN1327046C (en) | 2005-07-15 | 2005-07-15 | Monocrystalline Si3N4 nanometer belt and micro belt preparation method |
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| CN1769547A CN1769547A (en) | 2006-05-10 |
| CN1327046C true CN1327046C (en) | 2007-07-18 |
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| CN101648697B (en) * | 2009-07-17 | 2013-12-18 | 宁波工程学院 | Method for preparing nanobelt |
| CN104776945B (en) * | 2014-09-27 | 2018-08-24 | 宁波工程学院 | Silicon nitride nano band high sensibility pressure transducer |
| CN113955796B (en) * | 2021-12-03 | 2024-01-19 | 中材人工晶体研究院有限公司 | Preparation method of raw material for growth of relaxation ferroelectric single crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1134404A (en) * | 1995-04-25 | 1996-10-30 | 西南交通大学 | Preparation method of alpha-Si3N4 whisker |
| CN1587449A (en) * | 2004-07-29 | 2005-03-02 | 中国科学院山西煤炭化学研究所 | Process for preparing alpha-Si3N4 whisker |
-
2005
- 2005-07-15 CN CNB2005100121882A patent/CN1327046C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1134404A (en) * | 1995-04-25 | 1996-10-30 | 西南交通大学 | Preparation method of alpha-Si3N4 whisker |
| CN1587449A (en) * | 2004-07-29 | 2005-03-02 | 中国科学院山西煤炭化学研究所 | Process for preparing alpha-Si3N4 whisker |
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