CN1822331A - Method for preparing titanium silicide nano line by chemical gas phase deposition method - Google Patents
Method for preparing titanium silicide nano line by chemical gas phase deposition method Download PDFInfo
- Publication number
- CN1822331A CN1822331A CN 200510097001 CN200510097001A CN1822331A CN 1822331 A CN1822331 A CN 1822331A CN 200510097001 CN200510097001 CN 200510097001 CN 200510097001 A CN200510097001 A CN 200510097001A CN 1822331 A CN1822331 A CN 1822331A
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- CN
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- Prior art keywords
- ticl
- nano wire
- tisi
- sih
- titanium silicide
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 238000000034 method Methods 0.000 title claims abstract description 43
- 229910021341 titanium silicide Inorganic materials 0.000 title claims abstract description 15
- 239000000126 substance Substances 0.000 title abstract description 7
- 238000000151 deposition Methods 0.000 title description 4
- 239000002070 nanowire Substances 0.000 claims abstract description 53
- 229910008484 TiSi Inorganic materials 0.000 claims abstract description 34
- 239000010936 titanium Substances 0.000 claims abstract description 26
- 229910021332 silicide Inorganic materials 0.000 claims abstract description 14
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 8
- 239000000376 reactant Substances 0.000 claims abstract description 4
- 239000003085 diluting agent Substances 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 17
- 239000011521 glass Substances 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 17
- 239000012495 reaction gas Substances 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002912 waste gas Substances 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 abstract 2
- 229910003074 TiCl4 Inorganic materials 0.000 abstract 2
- 229910008479 TiSi2 Inorganic materials 0.000 abstract 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 abstract 2
- -1 TiSi2 compound Chemical class 0.000 abstract 1
- DFJQEGUNXWZVAH-UHFFFAOYSA-N bis($l^{2}-silanylidene)titanium Chemical compound [Si]=[Ti]=[Si] DFJQEGUNXWZVAH-UHFFFAOYSA-N 0.000 abstract 1
- 238000005137 deposition process Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 16
- 230000001143 conditioned effect Effects 0.000 description 9
- 238000004062 sedimentation Methods 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000007792 gaseous phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 229910019001 CoSi Inorganic materials 0.000 description 1
- 229910005883 NiSi Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- Silicon Compounds (AREA)
- Chemical Vapour Deposition (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Present invention discloses a method for preparing titanium silicide nano wire by chemical vapour deposition process. Said method adopts vapour deposition process using SiH4 and TiCl4 as reactant, using N2 as diluents and shielding gas atmosphere. Said method firstly form metal silicide (Ti 5Si3, TiSi2or Ti 5Si3and TiSi2 compound) thin layer, then to form high density silicide (TiSi, Ti 5 Si3 or TiSi2) nano wire. Nano wire diameter is between 10-40 nm, length between 10 micrometer, nano wire pattern can be controlled by changing technological conditions, nano wire chemical constitution can be controlled by changing mol ratio of reactant SiH4 / TiCl4.
Description
Technical field
The present invention relates to the technology of preparing of titanium silicide nano line.Relate in particular to is to form highdensity silicide nano wire fast by chemical gaseous phase depositing process on glass substrate.
Background technology
Along with the development of microelectric technique, the preparation of nano wire has in recent years caused extensive attention, and nano wire has a wide range of applications as the basic module in nanoelectronic and the optoelectronic fabrication techniques.The application of nano material in semiconductor technology can obtain higher device density, and this is that conventional semiconductor technology is incomparable.Metal silicide is widely used in modern semiconductor technology in the middle of the manufacturing of the door, source/drain electrode of metal-oxide semiconductor (MOS) (MOS) device, mos field effect transistor (MOSFET), dynamic random access memory (DRAM) among the ULSI and interconnected, ohmic contact.Along with constantly reducing of device size in microelectric technique, the metal silicide nano-wire of many one dimension sizes has prepared.He etc. have prepared CoSi
2Nano wire, Chen etc. have prepared ErSi
2Nano wire, Lee etc. have been prepared the NiSi nano wire, and Luo etc. have prepared Pt
6Si
5Nano wire, Ragana etc. have been prepared extension rare metal silicide nano wire, but these nano wires all form by physical gas-phase deposite method, mainly are sputtering methods.This method yields poorly to the requirement height of equipment.For having overcome the shortcoming of method for preparing metal silicide nano-wire, we have successfully prepared the titanium silicide nano line by chemical gaseous phase depositing process, this is a kind of new method of growing metal silicide nano wire, this method both can be applicable to the preparation of various metal silicide nano-wires, can be used for the preparation of various inorganic compound nano wires again.
Summary of the invention
The object of the present invention is to provide a kind of chemical vapour deposition technique to prepare the method for titanium silicide nano line.
The technical solution adopted for the present invention to solve the technical problems is that the step of this method is as follows:
1) reactant is SiH
4And TiCl
4, with N
2Be diluent gas and protective atmosphere;
2) TiCl
4Constant temperature is at 30～60 ℃; TiCl
4Pipeline heat insulation to 40～70 ℃ of process;
3) by gas generator, use N
2Carry TiCl
4
4) SiH
4, TiCl
4And N
2Mix at mixing chamber; Each road gas equates that at the pressure of mixing chamber porch pressure remains between 111325～131325Pa;
5) molar concentration of each material in the overall reaction gas:
a)SiH
4：0.33～5％；
b)TiCl
4：0.33～1.67％；
C) SiH
4: TiCl
4Mol ratio: 1～3;
6) growing system is a quartz tube reactor, and growing system pressure is 101325～121325Pa;
7) glass substrate places in the quartz tube reactor and carries out, and the glass substrate temperature is 690～750 ℃, SiH
4, TiCl
4And N
2Mixed gas delivery is reacted to glass substrate, and the reaction time is 30～300 seconds, generates the titanium silicide thin layer on glass substrate earlier, forms highdensity silicide nano wire then on this metal silicide film;
8) waste gas is handled the back discharging through absorbing.
Described film is Ti
5Si
3, TiSi
2Or Ti
5Si
3With TiSi
2Compound.Described nano wire is TiSi, Ti
5Si
3Or TiSi
2Described nano wire is a monocrystal nanowire.The diameter of described nano wire is between 10～40nm, and length is at 0.2～10 μ m.
The present invention compares the beneficial effect that has with background technology:
1, be equipped with metal silicide nano-wire with the CVD legal system, this method is low for equipment requirements, but output is big, the efficient height.Than existing physical gas-phase deposite method bigger superiority is arranged;
2, this method is not used template and catalyst, fast a large amount of generations the titanium silicide nano line of monocrystalline;
3, by preparation condition is changed, can obtain the nano wire of various patterns;
4,, can obtain the nano wire of various chemical compositions by change to preparation feedback thing mol ratio.
Description of drawings
Fig. 1 nanowire growth schematic diagram of the present invention;
The scanning electron microscopy profile of the TiSi nano wire sample of Fig. 2 embodiment 1 preparation;
The scanning electron microscope diagram of the TiSi nano wire of Fig. 3 embodiment 2 preparations;
The high resolution transmission electron microscopy figure and the electron diffraction diagram of the TiSi nano wire of Fig. 4 embodiment 2 preparations.
Embodiment
As shown in Figure 1, on common glass substrates 1, deposition thin film 2 forms titanium silicide nano line 3 then on this film 2 earlier.
Described film is Ti
5Si
3, TiSi
2Or Ti
5Si
3With TiSi
2Compound.Described nano wire is TiSi, Ti
5Si
3Or TiSi
2Described nano wire is a monocrystal nanowire.The diameter of described nano wire is between 10～40nm, and length is at 0.2～10 μ m.
Be embodiments of the invention below:
690 ℃ of reaction temperatures, TiCl
4Constant temperature is at 60 ℃, TiCl
4The pipeline heat insulation to 70 ℃ of process, conditioned reaction gas SiH
4: TiCl
4Mol ratio is 1, SiH
4: 1.67%, TiCl
4: 1.67%, N
2: 96.66%, the pressure of each road gas in the mixing chamber porch is 111325Pa, growing system pressure maintains 101325Pa, about 120 seconds of sedimentation time.On glass substrate, form Ti
5Si
3Film and TiSi monocrystal nanowire.The results are shown in subordinate list and shown in Figure 2.
690 ℃ of reaction temperatures, TiCl
4Constant temperature is at 40 ℃, TiCl
4The pipeline heat insulation to 50 ℃ of process, conditioned reaction gas SiH
4: TiCl
4Mol ratio is 1, SiH
4: 1%, TiCl
4: 1%, N
2: 98%, the pressure of each road gas in the mixing chamber porch is 111325Pa, growing system pressure maintains 101325Pa, about 300 seconds of sedimentation time.On glass substrate, form Ti
5Si
3Film and TiSi monocrystal nanowire.The results are shown in shown in subordinate list and Fig. 3～4.
690 ℃ of reaction temperatures, TiCl
4Constant temperature is at 30 ℃, TiCl
4The pipeline heat insulation to 40 ℃ of process, conditioned reaction gas SiH
4: TiCl
4Mol ratio is 1, SiH
4: 0.33%, TiCl
4: 0.33%, N
2: 99.34%, the pressure of each road gas in the mixing chamber porch is 111325Pa, growing system pressure maintains 101325Pa, about 210 seconds of sedimentation time.On glass substrate, form Ti
5Si
3Film and TiSi monocrystal nanowire.The results are shown in subordinate list.
Embodiment 4
700 ℃ of reaction temperatures, TiCl
4Constant temperature is at 40 ℃, TiCl
4The pipeline heat insulation to 50 ℃ of process, conditioned reaction gas SiH
4: TiCl
4Mol ratio is 2, SiH
4: 3%, TiCl
4: 1.5%, N
2: 95.5%, the pressure of each road gas in the mixing chamber porch is 121325Pa, growing system pressure maintains 111325Pa, about 120 seconds of sedimentation time.On glass substrate, form Ti
5Si
3Film and Ti
5Si
3Monocrystal nanowire.The results are shown in subordinate list.
Embodiment 5
700 ℃ of reaction temperatures, TiCl
4Constant temperature is at 60 ℃, TiCl
4The pipeline heat insulation to 70 ℃ of process, conditioned reaction gas SiH
4: TiCl
4Mol ratio is 3, SiH
4: 5%, TiCl
4: 1.67%, N
2: 93.33%, the pressure of each road gas in the mixing chamber porch is 121325Pa, growing system pressure maintains 111325Pa, about 30 seconds of sedimentation time.On glass substrate, form TiSi
2Film and TiSi
2Monocrystal nanowire.The results are shown in subordinate list.
Embodiment 6
690 ℃ of reaction temperatures, TiCl
4Constant temperature is at 40 ℃, TiCl
4The pipeline heat insulation to 50 ℃ of process, conditioned reaction gas SiH
4: TiCl
4Mol ratio is 3, SiH
4: 1.5%, TiCl
4: 0.5%, N
2: 98%, about 60 seconds of sedimentation time, the pressure of each road gas in the mixing chamber porch is 131325Pa, growing system pressure maintains 121325Pa.On glass substrate, form TiSi
2Film.Then, conditioned reaction gas SiH
4/ TiCl
4Mol ratio is 1, SiH
4: 1%, TiCl
4: 1%, N
2: 98%, about 90 seconds of sedimentation time, the pressure of each road gas in the mixing chamber porch is 131325Pa, growing system pressure maintains 121325Pa.At TiSi
2Form the TiSi monocrystal nanowire on the film.The results are shown in subordinate list.
Embodiment 7
750 ℃ of reaction temperatures, TiCl
4Constant temperature is at 40 ℃, TiCl
4The pipeline heat insulation to 50 ℃ of process, conditioned reaction gas SiH
4: TiCl
4Mol ratio is 1, SiH
4: 1%, TiCl
4: 1%, N
2: 98%, about 40 seconds of sedimentation time, the pressure of each road gas in the mixing chamber porch is 131325Pa, growing system pressure maintains 121325Pa.On glass substrate, form Ti
5Si
3Film.Then, conditioned reaction gas SiH
4/ TiCl
4Mol ratio is 2, SiH
4: 2%, TiCl
4: 1%, N
2: 97%, about 80 seconds of sedimentation time, the pressure of each road gas in the mixing chamber porch is 131325Pa, growing system pressure maintains 121325Pa.At Ti
5Si
3Form TiSi on the film
2Monocrystal nanowire.The results are shown in subordinate list.
The sign of subordinate list film
| Example | Crystalline phase in the film | The chemical composition of nano wire | Atomic ratio Ti: Si in the nano wire | The diameter of nano wire (nm) | The length of nano wire (μ m) |
| Example 1 | Ti 5Si 3 | TiSi | 1∶1.1 | 20 | 0.5 |
| Example 2 | Ti 5Si 3 | TiSi | 1∶1.05 | 15～25 | 5～10 |
| Example 3 | Ti 5Si 3 | TiSi | 1∶1.07 | 15～25 | 0.2 |
| Example 4 | Ti 5Si 3，TiSi 2 | Ti 5Si 3 | 1∶0.64 | 15～20 | 2～3 |
| Example 5 | TiSi 2 | TiSi 2 | 1∶2.1 | 10～25 | 3～5 |
| Example 6 | TiSi 2 | TiSi | 1∶1.1 | 20～40 | 0.5～1 |
| Example 7 | Ti 5Si 3 | TiSi 2 | 1∶2.15 | 15～25 | 3～4 |
Crystalline phase is tested with X-ray diffractometer in the film.
The chemical composition of nano wire is by X-ray diffractometer and electronic diffraction test
The diameter of nano wire and length are by scanning electron microscopy and transmission electron microscope test.
Contained element and ratio thereof are tested by the X ray energy dispersive spectrometry.
Claims (5)
1, a kind of chemical vapour deposition technique prepares the method for titanium silicide nano line, it is characterized in that the step of this method is as follows:
1) reactant is SiH
4And TiCl
4, with N
2Be diluent gas and protective atmosphere;
2) TiCl
4Constant temperature is at 30～60 ℃; TiCl
4Pipeline heat insulation to 40～70 ℃ of process;
3) by gas generator, use N
2Carry TiCl
4
4) SiH
4, TiCl
4And N
2Mix at mixing chamber; Each road gas equates that at the pressure of mixing chamber porch pressure remains between 111325～131325Pa;
5) molar concentration of each material in the overall reaction gas:
a)SiH
4：0.33～5％；
b)TiCl
4：0.33～1.67％；
C) SiH
4: TiCl
4Mol ratio: 1～3;
6) growing system is a quartz tube reactor, and growing system pressure is 101325～121325Pa;
7) glass substrate places in the quartz tube reactor and carries out, and the glass substrate temperature is 690～750 ℃, SiH
4, TiCl
4And N
2Mixed gas delivery is reacted to glass substrate, and the reaction time is 30～300 seconds, generates the titanium silicide thin layer on glass substrate earlier, forms highdensity silicide nano wire then on this metal silicide film;
8) waste gas is handled the back discharging through absorbing.
2, a kind of chemical vapour deposition technique according to claim 1 prepares the method for titanium silicide nano line, it is characterized in that: described film is Ti
5Si
3, TiSi
2Or Ti
5Si
3With TiSi
2Compound.
3, a kind of chemical vapour deposition technique according to claim 1 prepares the method for titanium silicide nano line, it is characterized in that: described nano wire is TiSi, Ti
5Si
3Or TiSi
2
4, a kind of chemical vapour deposition technique according to claim 1 prepares the method for titanium silicide nano line, it is characterized in that: described nano wire is a monocrystal nanowire.
5, a kind of chemical vapour deposition technique according to claim 1 prepares the method for titanium silicide nano line, it is characterized in that: the diameter of described nano wire is between 10～40nm, and length is at 0.2～10 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100970013A CN100356522C (en) | 2005-12-31 | 2005-12-31 | Method for preparing titanium silicide nano line by chemical gas phase deposition method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100970013A CN100356522C (en) | 2005-12-31 | 2005-12-31 | Method for preparing titanium silicide nano line by chemical gas phase deposition method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1822331A true CN1822331A (en) | 2006-08-23 |
| CN100356522C CN100356522C (en) | 2007-12-19 |
Family
ID=36923530
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100970013A Expired - Fee Related CN100356522C (en) | 2005-12-31 | 2005-12-31 | Method for preparing titanium silicide nano line by chemical gas phase deposition method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100356522C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102400220A (en) * | 2011-12-02 | 2012-04-04 | 南昌大学 | Method for preparing titanium oxide nano wire with self-induction chemical vapor deposition method |
| US8158254B2 (en) | 2008-08-25 | 2012-04-17 | The Trustees Of Boston College | Methods of fabricating complex two-dimensional conductive silicides |
| US8216436B2 (en) | 2008-08-25 | 2012-07-10 | The Trustees Of Boston College | Hetero-nanostructures for solar energy conversions and methods of fabricating same |
| RU2629121C1 (en) * | 2016-07-18 | 2017-08-24 | Федеральное государственное бюджетное научное учреждение "Федеральный исследовательский центр "Красноярский научный центр Сибирского отделения Российской академии наук" | Method for titanium silicides production |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5240739A (en) * | 1992-08-07 | 1993-08-31 | Micron Technology | Chemical vapor deposition technique for depositing titanium silicide on semiconductor wafers |
| CN1294098C (en) * | 2005-05-25 | 2007-01-10 | 浙江大学 | Titanium silicide coated glass with compound functions prepared by nitrogen protection under normal pressure and preparation method thereof |
-
2005
- 2005-12-31 CN CNB2005100970013A patent/CN100356522C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8158254B2 (en) | 2008-08-25 | 2012-04-17 | The Trustees Of Boston College | Methods of fabricating complex two-dimensional conductive silicides |
| US8216436B2 (en) | 2008-08-25 | 2012-07-10 | The Trustees Of Boston College | Hetero-nanostructures for solar energy conversions and methods of fabricating same |
| CN102400220A (en) * | 2011-12-02 | 2012-04-04 | 南昌大学 | Method for preparing titanium oxide nano wire with self-induction chemical vapor deposition method |
| CN102400220B (en) * | 2011-12-02 | 2014-04-09 | 南昌大学 | Method for preparing titanium oxide nano wire with self-induction chemical vapor deposition method |
| RU2629121C1 (en) * | 2016-07-18 | 2017-08-24 | Федеральное государственное бюджетное научное учреждение "Федеральный исследовательский центр "Красноярский научный центр Сибирского отделения Российской академии наук" | Method for titanium silicides production |
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| Publication number | Publication date |
|---|---|
| CN100356522C (en) | 2007-12-19 |
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