CN115537928A - Silicon nitride single crystal material and preparation method thereof - Google Patents
Silicon nitride single crystal material and preparation method thereof Download PDFInfo
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- CN115537928A CN115537928A CN202211138651.8A CN202211138651A CN115537928A CN 115537928 A CN115537928 A CN 115537928A CN 202211138651 A CN202211138651 A CN 202211138651A CN 115537928 A CN115537928 A CN 115537928A
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- Prior art keywords
- silicon nitride
- single crystal
- crystal material
- nitride single
- inert gas
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 45
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000013078 crystal Substances 0.000 title claims abstract description 41
- 239000000463 material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 66
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims abstract description 43
- 239000011261 inert gas Substances 0.000 claims abstract description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000919 ceramic Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000012495 reaction gas Substances 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 5
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 description 7
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001709 polysilazane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/38—Nitrides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
Abstract
The invention discloses a silicon nitride single crystal material and a preparation method thereof, relating to the technical field of silicon nitride single crystals and comprising the following steps of 10: putting a monocrystalline silicon wafer into a ceramic boat, putting the ceramic boat into a heating furnace, and introducing inert gas; step 20, heating and keeping constant temperature: gradually raising the temperature of the heating furnace to 1150-1350 ℃, and keeping the temperature for 2-10h; step 30, heating reaction: in the continuous heating process, introducing constant reaction gas flow inert gas and nitrogen in a mass ratio of 10; step 40, epitaxial growth: the method comprises the steps of selecting ammonia gas as pretreatment gas, cleaning the surface of the monocrystalline silicon wafer at high temperature, removing an oxide layer formed on the surface of the monocrystalline silicon wafer, and facilitating the generation of the silicon nitride crystal by means of chemical vapor deposition.
Description
Technical Field
The invention relates to the technical field of silicon nitride single crystals, in particular to a silicon nitride single crystal material and a preparation method thereof.
Background
Silicon nitride is an artificially synthesized single crystal material, and has excellent performances of high temperature resistance, high strength, high modulus, low density, good chemical stability and the like, so that the silicon nitride has wide application in the fields of ceramics, microelectronics, space science and the like. With the continuous development of science and technology, people develop a great deal of research on the properties of silicon nitride powder materials, crystal materials, bulk sintering material film materials and the like.
In recent years, a silicon nitride single crystal material is researched, polysilazane is filled with nitrogen at high temperature for crosslinking and curing for half an hour in a low-temperature crosslinking and curing mode to obtain semi-transparent non-static solid SiCN, the SiCN is mixed with a metal element catalyst grinding component in a high-temperature pyrolysis mode and then is put on an alumina ceramic substrate for high-temperature pyrolysis, and then the mixture is cooled to room temperature, the whole process is protected by nitrogen to obtain silicon nitride single crystal, and the silicon nitride single crystal line is obtained through the anisotropic structure of silicon nitride and by the anisotropic oriented growth characteristic.
In addition, metal elements are introduced as catalysts to reduce the purity of the silicon nitride, and simultaneously great difficulty and complex process are caused to purification, so that a simple preparation method of the silicon nitride single crystal material is needed.
Disclosure of Invention
Technical problem to be solved
The invention provides a silicon nitride single crystal material and a preparation method thereof, aiming at the defects of the prior art, the invention takes optimized ammonia gas as pretreatment gas, cleans the surface of a single crystal silicon wafer at high temperature, removes an oxide layer formed on the surface of the single crystal silicon wafer, and is convenient for promoting the generation of silicon nitride crystals in a chemical vapor deposition mode.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a silicon nitride single crystal material comprises the following steps:
step 10, providing a monocrystalline silicon wafer substrate: placing a monocrystalline silicon wafer into a ceramic boat, placing the ceramic boat into a heating furnace, and introducing inert gas;
step 20, heating and keeping constant temperature: gradually raising the temperature of the heating furnace to 1150-1350 ℃, and keeping the temperature for 2-10h;
step 30, heating reaction: in the continuous heating process, introducing constant reaction gas flow inert gas and nitrogen in a mass ratio of 10;
step 40, epitaxial growth: and after the heating furnace is cooled to room temperature, white floccules are formed on the surface of the recrystallized silicon wafer, and the silicon nitride single crystal material is obtained through mechanical glass.
Preferably, the monocrystalline silicon wafer is a porous sheet, the thickness of the monocrystalline silicon wafer is 0.5-5nm, the inert gas comprises argon, ammonia gas and hydrogen gas, preferably ammonia gas, and the inert gas is introduced in the step 10 to remove oxygen in the heating furnace.
Preferably, the heating furnace is heated at a heating rate of 25-35 ℃/min.
Preferably, the step 10 is performed for pretreating a single crystal silicon wafer.
Preferably, the pretreatment comprises the steps of introducing inert gas into a heating furnace and cleaning the surface of the monocrystalline silicon piece at 800-1000 ℃ for 5-10min.
Preferably, the nitrogen and the inert gas in step 30 are both high-purity gases, and the purity is 99.99-99.9999%.
Preferably, a silicon nitride single crystal material obtained by the process of claim 1.
(III) advantageous effects
The invention provides a silicon nitride single crystal material and a preparation method thereof, and the silicon nitride single crystal material has the following beneficial effects:
(1) According to the method, ammonia gas is preferably selected as pretreatment gas, the surface of the monocrystalline silicon piece is cleaned at high temperature, an oxide layer formed on the surface of the monocrystalline silicon piece is removed, and the generation of the silicon nitride crystal is facilitated in a chemical vapor deposition mode.
(2) The invention introduces the inert gas before the heating of the heating furnace in order to remove the residual oxygen and the like in the hearth, carries out the nitridation pretreatment in the atmosphere of ammonia gas, can quickly heat up, A large number of silicon nitride nuclei are covered on the surface of the monocrystalline silicon piece, and the generated silicon nitride crystal continues to grow and develop along the monocrystalline direction along with continuous heating, so that the nitriding speed of the monocrystalline silicon piece is increased, and the nitriding period is shortened.
(3) The preparation method has the advantages of simple process, low cost and relatively long period, and is favorable for large-scale production.
Detailed Description
All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
The invention provides a technical scheme that: a preparation method of a silicon nitride single crystal material comprises the following steps:
step 10, providing a monocrystalline silicon wafer substrate: placing a monocrystalline silicon wafer with the thickness of 0.5-1.5nm into a ceramic boat, placing the ceramic boat into a heating furnace, introducing inert gas, and removing oxygen in the heating furnace, wherein the inert gas comprises argon, ammonia and hydrogen, and preferably ammonia;
the method comprises the following steps of putting a monocrystalline silicon wafer into a heating furnace, introducing inert gas, cleaning the surface of the monocrystalline silicon wafer for 4-6min at 800 ℃, and removing an oxide layer formed on the surface of the monocrystalline silicon wafer.
Step 20, heating and keeping constant temperature: gradually raising the temperature of the heating furnace to 1150 ℃ at the heating rate of 25 ℃/min, and keeping the constant temperature for 2h;
step 30, heating reaction: in the continuous heating process, introducing constant reaction gas flow inert gas and nitrogen in a mass ratio of 10;
step 40, epitaxial growth: and after the heating furnace is cooled to room temperature, white floccules are formed on the surface of the recrystallized silicon wafer, and the silicon nitride single crystal material is obtained through mechanical glass.
Example 2
The invention provides a technical scheme that: a preparation method of a silicon nitride single crystal material comprises the following steps:
step 10, providing a monocrystalline silicon wafer substrate: placing a monocrystalline silicon wafer with the thickness of 1.5-2.5nm into a ceramic boat, placing the ceramic boat into a heating furnace, and introducing inert gas to remove oxygen in the heating furnace, wherein the inert gas is one or more of argon, ammonia and hydrogen;
wherein, after the monocrystalline silicon piece is placed in a heating furnace, inert gas is introduced into the heating furnace, the monocrystalline silicon piece is cleaned for 6-8min at 900 ℃, and the purpose is to remove an oxide layer formed on the surface of the monocrystalline silicon piece.
Step 20, heating and keeping constant temperature: gradually raising the temperature of the heating furnace to 1200 ℃ at the heating rate of 30 ℃/min, and keeping the constant temperature for 6h;
step 30, heating reaction: in the continuous heating process, introducing constant reaction gas flow inert gas and nitrogen in a mass ratio of 10;
step 40, epitaxial growth: and after the heating furnace is cooled to the room temperature, white floccules are formed on the surface of the recrystallized silicon wafer, and the silicon nitride single crystal material is obtained through mechanical glass.
Example 3
The invention provides a technical scheme that: a preparation method of a silicon nitride single crystal material comprises the following steps:
step 10, providing a monocrystalline silicon wafer substrate: placing a monocrystalline silicon wafer with the thickness of 2.5-3.5nm into a ceramic boat, placing the ceramic boat into a heating furnace, introducing inert gas, and removing oxygen in the heating furnace, wherein the inert gas comprises one or more than two of argon, ammonia and hydrogen;
the method comprises the following steps of putting a monocrystalline silicon wafer into a heating furnace, introducing inert gas, cleaning the surface of the monocrystalline silicon wafer for 8-10min at 1000 ℃, and removing an oxide layer formed on the surface of the monocrystalline silicon wafer.
Step 20, heating and keeping constant temperature: gradually raising the temperature of the heating furnace to 1350 ℃ at the heating rate of 35 ℃/min, and keeping the constant temperature for 10 hours;
step 30, heating reaction: introducing constant reaction gas flow inert gas and nitrogen in the continuous heating process, wherein the mass ratio of inert gas to nitrogen is 10;
step 40, epitaxial growth: and after the heating furnace is cooled to room temperature, white floccules are formed on the surface of the recrystallized silicon wafer, and the silicon nitride single crystal material is obtained through mechanical glass.
Example 4
The invention provides a technical scheme that: a preparation method of a silicon nitride single crystal material comprises the following steps:
step 10, providing a monocrystalline silicon wafer substrate: placing a monocrystalline silicon wafer with the thickness of 3.5-5nm into a ceramic boat, placing the ceramic boat into a heating furnace, introducing inert gas, and removing oxygen in the heating furnace, wherein the inert gas comprises one or more than two of argon, ammonia and hydrogen;
wherein, after the monocrystalline silicon piece is placed in a heating furnace, inert gas is introduced into the heating furnace, the monocrystalline silicon piece is cleaned for 10-12min at 900 ℃, and the purpose is to remove an oxide layer formed on the surface of the monocrystalline silicon piece.
Step 20, heating and keeping constant temperature: gradually raising the temperature of the heating furnace to 1200 ℃ at the heating rate of 30 ℃/min, and keeping the constant temperature for 6h;
step 30, heating reaction: introducing constant reaction gas flow inert gas and nitrogen in the continuous heating process, wherein the mass ratio of inert gas to nitrogen is 10;
step 40, epitaxial growth: and after the heating furnace is cooled to room temperature, white floccules are formed on the surface of the recrystallized silicon wafer, and the silicon nitride single crystal material is obtained through mechanical glass.
The working principle is as follows:
in summary, according to the preparation method of the silicon nitride single crystal material, ammonia gas is preferably selected as pretreatment gas, the surface of the single crystal silicon wafer is cleaned at high temperature, an oxide layer formed on the surface of the single crystal silicon wafer is removed, and the silicon nitride crystal is convenient to generate through a chemical vapor deposition mode.
It is noted that, in this document, relational terms such as first and second, and the like, if any, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising a," "8230," "8230," or "comprising" does not exclude the presence of additional like elements in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A preparation method of a silicon nitride single crystal material is characterized by comprising the following steps: the method comprises the following steps:
step 10, providing a monocrystalline silicon wafer substrate: putting a monocrystalline silicon wafer into a ceramic boat, putting the ceramic boat into a heating furnace, and introducing inert gas;
step 20, heating and keeping constant temperature: gradually raising the temperature of the heating furnace to 1150-1350 ℃, and keeping the temperature for 2-10h;
step 30, heating reaction: introducing constant reaction gas flow inert gas and nitrogen in the continuous heating process, wherein the mass ratio of inert gas to nitrogen is 10;
step 40, epitaxial growth: and after the heating furnace is cooled to room temperature, white floccules are formed on the surface of the recrystallized silicon wafer, and the silicon nitride single crystal material is obtained through mechanical glass.
2. The method for producing a silicon nitride single crystal material according to claim 1, wherein: the monocrystalline silicon piece is a porous sheet, the thickness of the monocrystalline silicon piece is 0.5-5nm, the inert gas comprises argon, ammonia gas and hydrogen gas, preferably ammonia gas, and the inert gas is introduced in the step 10 to remove oxygen in the heating furnace.
3. The method for producing a silicon nitride single crystal material according to claim 1, wherein: the heating furnace is heated at a heating rate of 25-35 ℃/min.
4. The method for producing a silicon nitride single crystal material according to claim 1, wherein: the step 10 is to pre-treat a single crystal silicon wafer.
5. The method for producing a silicon nitride single crystal material according to claim 4, wherein: and introducing inert gas into the heating furnace and cleaning the surface of the monocrystalline silicon wafer at 800-1000 ℃ for 5-10min.
6. The method for producing a silicon nitride single crystal material according to claim 1, wherein: the nitrogen and the inert gas in the step 30 are both high-purity gases, and the purity is 99.99-99.9999%.
7. A silicon nitride single crystal material characterized by: the silicon nitride single crystal material is obtained by the steps of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211138651.8A CN115537928A (en) | 2022-09-19 | 2022-09-19 | Silicon nitride single crystal material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211138651.8A CN115537928A (en) | 2022-09-19 | 2022-09-19 | Silicon nitride single crystal material and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN115537928A true CN115537928A (en) | 2022-12-30 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101603207A (en) * | 2009-07-21 | 2009-12-16 | 中国地质大学（北京） | The preparation method of network branched silicon nitride single crystal nanostructure with high purity and high yield |
| CN104891456A (en) * | 2015-06-04 | 2015-09-09 | 中国人民解放军国防科学技术大学 | One-dimensional alpha-Si3N4 nano material and preparation method thereof |
| CN110357051A (en) * | 2019-07-09 | 2019-10-22 | 南昌大学 | A kind of preparation method of monocrystalline α phase silicon nitride nano whisker |
| CN110436934A (en) * | 2019-07-09 | 2019-11-12 | 南昌大学 | A kind of preparation method of alpha-phase silicon nitride powder, overlength beta-silicon nitride nanowire |
| CN113122925A (en) * | 2021-04-21 | 2021-07-16 | 中国科学院苏州纳米技术与纳米仿生研究所 | Silicon nitride single crystal and preparation method and application thereof |
-
2022
- 2022-09-19 CN CN202211138651.8A patent/CN115537928A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101603207A (en) * | 2009-07-21 | 2009-12-16 | 中国地质大学（北京） | The preparation method of network branched silicon nitride single crystal nanostructure with high purity and high yield |
| CN104891456A (en) * | 2015-06-04 | 2015-09-09 | 中国人民解放军国防科学技术大学 | One-dimensional alpha-Si3N4 nano material and preparation method thereof |
| CN110357051A (en) * | 2019-07-09 | 2019-10-22 | 南昌大学 | A kind of preparation method of monocrystalline α phase silicon nitride nano whisker |
| CN110436934A (en) * | 2019-07-09 | 2019-11-12 | 南昌大学 | A kind of preparation method of alpha-phase silicon nitride powder, overlength beta-silicon nitride nanowire |
| CN113122925A (en) * | 2021-04-21 | 2021-07-16 | 中国科学院苏州纳米技术与纳米仿生研究所 | Silicon nitride single crystal and preparation method and application thereof |
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