CN109721056A - The method that depth removes impurity element in high-purity silicon carbide powder - Google Patents
The method that depth removes impurity element in high-purity silicon carbide powder Download PDFInfo
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- CN109721056A CN109721056A CN201910152688.8A CN201910152688A CN109721056A CN 109721056 A CN109721056 A CN 109721056A CN 201910152688 A CN201910152688 A CN 201910152688A CN 109721056 A CN109721056 A CN 109721056A
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Abstract
The method that depth removes impurity element in high-purity silicon carbide powder, it is related to the Industrialized processing technique field of HIGH-PURITY SILICON and high-purity carbon high-temperature synthesis production high-purity silicon carbide that high-purity silicon source/carbon source obtains, the especially deep purification method of manufacturing silicon carbide semiconductor high-purity silicon carbide.The characteristic volatilized using the high temperature difficulty of silicon carbide, under conditions of 900~1200 DEG C, low-boiling chloride is generated with HCl gas containing impurity element boron, aluminium, iron, titanium, vanadium in miscellaneous silicon carbide powder etc. and is evaporated, to reduce the content containing impurity elements such as boron, aluminium, iron, titanium, vanadium in miscellaneous silicon carbide powder, the method that the impurity elements such as boron, aluminium, titanium, iron, vanadium in the silicon carbide powder of certain high-purity are already expired in depth removal is realized with this, to promote the quality of high-purity silicon carbide powder, the yield for single-crystal silicon carbide is improved.
Description
Technical field
HIGH-PURITY SILICON and high-purity carbon high-temperature synthesis the production high-purity silicon carbide obtained the present invention relates to high-purity silicon source/carbon source
The deep purification method of Industrialized processing technique field, especially manufacturing silicon carbide semiconductor high-purity silicon carbide (5N+).
Background technique
Manufacturing silicon carbide semiconductor is new three generations's wide bandgap semiconductor.Most of semiconductor material is all monocrystalline silicon at present, and
Monocrystalline silicon carbide has many superior physical characteristics, such as about 10 times of electric field strength, about high 3 times of heat than monocrystalline silicon
Conductance, about wide 3 times of forbidden bandwidths, the saturation drift velocity about to double, and carbofrax material is to the energy consumption pole of electric power
It is low, the 21 century ideal semiconductor material for being much better than monocrystalline silicon is become, the forward position commanding elevation of global semiconductor industry is become.
Because of these features, it can be used under extreme environmental condition with the device that SiC makes, microwave and high frequency and shortwave
Long device is application market mature at present.And in military phased-array radar, communication broadcasting system, with SiC as lining
The brightness blue light LED at bottom is then the Primary Component of Panchromatic great-arear display screen.
As emerging strategic guiding industry, silicon carbide is the key basic material for developing the 3rd generation semiconductor industry, the world
Developed country's actively investment research and development and industrialized development.
Third generation semiconductor crystal wafer manufacturing enterprise, China has formd certain international competitiveness.But the height as raw material
The preparation process condition of pure SiC powder is extremely harsh, and hardware and detection and analysis require height, but current bottleneck is can not to produce
Purity be 5~6N(99.9999%) SiC raw material.
Summary of the invention
Object of the present invention is to propose that one kind can the impurity member such as boron, aluminium, titanium, iron, vanadium in depth removal high-purity silicon carbide powder
Element, the silicon carbide purity after making removal of impurities reach the method for 5~6N.
The technical scheme is that: being passed through temperature with HCl gas is 900~1200 DEG C containing miscellaneous silicon carbide powder, makes to contain
Impurity element in miscellaneous silicon carbide powder is reacted with HCl generates low-boiling chloride, and the low-boiling chloride of generation is arranged
Out, unreacted solid is collected, i.e. the purity silicon carbide powder that is 5~6N.
The present invention utilizes the characteristic of the high temperature difficulty volatilization (2700 DEG C of fusing point, distil) of silicon carbide, in 900~1200 DEG C of item
Under part, low-boiling chloride is generated with HCl gas containing impurity element boron, aluminium, iron, titanium, vanadium in miscellaneous silicon carbide powder etc. and is steamed
It issues, to reduce the content containing impurity elements such as boron, aluminium, iron, titanium, vanadium in miscellaneous silicon carbide powder, depth is realized with this
The method that the impurity elements such as boron, aluminium, titanium, iron, vanadium in the silicon carbide powder of certain high-purity are already expired in degree removal.
Reactional equation and product boiling point of the present invention is as follows:
The present invention utilizes HCL gas critical impurities element boron brilliant with silicon carbide length is influenced at a certain temperature, aluminium, iron, titanium, vanadium
Generating low-boiling chloride enables the impurity elements depth such as boron, aluminium, iron, titanium, vanadium to remove, to promote high-pure SiC power
The quality of body, the yield for single-crystal silicon carbide are improved.
Further, HCl gas flow of the present invention is 2~3L/min.It is impurity member in high-purity silicon carbide powder
Cellulose content is few, and (PPM grades, removed impurity element is less than 2PPM before depth purifies, i.e., less than 0.0002%), required HCL participates in reaction
Amount it is few, therefore flow is set as 2~3L/min of low discharge, while can reduce flow velocity, increases and is detained the reaction time, reduces HCL and uses
Amount.
The present invention will be loaded into high-purity silica pot containing miscellaneous silicon carbide powder to react, to reduce other impurity
It brings into.
Confirm through repetition test: the thickness of silicon carbide materials filling is thinner, and the effect of impurity is better, therefore the present invention also proposes
Containing miscellaneous silicon carbide powder with a thickness of 1~8cm.More preferably containing miscellaneous silicon carbide powder with a thickness of 2cm.
Above-mentioned reaction carries out under 3~5mmHg pressure condition.The pressure is minute-pressure, keeps quartzy pipe pressure close in minute-pressure
In normal pressure state, external stress is small, guarantees quartz ampoule service life.
The above reaction time is 2~4 hours.As the reaction time is less than 1 hour hereinafter, impurity removes unobvious, same row
Miscellaneous time extends, and after being greater than 4 hours, impurity content does not decline further.It was advisable according to removal efficiency situation 2~4 hours.
The low-boiling chloride of generation is absorbed in lye, low boiling point chloride can be through spray equipment with HCL gas
Into lye, centralized collection does fixed-end forces after reaching a certain concentration.
Pass through packing layer in the lye ullage for collecting chloride (filler is polyhedron empty ball plastic sphere).Through
Packing layer is crossed, tail gas containing HCl and lye absorbing liquid carry out gas-liquid two-phase and come into full contact with absorption neutralization reaction, and tail gas is after purification
It is discharged into atmosphere.Lye absorbing liquid tower bottom after water pump is pressurized tower top spray and under, be finally back to tower bottom recycling.
In order to further prevent reaction member to bring impurity into, silica crucible of the present invention is placed in quartz ampoule.
Similarly, the flow plug of the silica crucible periphery setting quartz material in the quartz ampoule.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the invention.
Specific embodiment
One, the explanation of process units:
As shown in Figure 1, the present invention is mainly made of quartz ampoule 1, Guan Cha bottle 3, spray equipment 4.
1 peripheral hardware heating jacket 8 of quartz ampoule, heating jacket 8 wrap up insulating layer 9 outside.Silica crucible 2 and two built in quartz ampoule 1
The flow plug 11,12 of group quartz material, flow plug 11 are arranged between the end and crucible 2 of connection HCl steel cylinder 5 of quartz ampoule 1
1 internal channel of quartz ampoule on, flow plug 12 be arranged in quartz ampoule 1 connection Guan Cha bottle 3 and crucible 2 between quartz ampoule 1 in lead to
On road.
Flow plug 11,12 is respectively by one piece of quartz plate compatible with 1 cross section of inboard wall of quartz ampoule and several quartz ampoule groups
At opening up hole on quartz plate, quartz ampoule is placed and is fixed in each hole.
Crucible 2 is for putting into carborundum powder 10 when production, and flow plug 11,12 are used to disperse in HCl air-flow, flow velocity drop
It is low, increase the residence time in quartz ampoule, is come into full contact with high-purity silicon carbide powder, reduce the amount of escaping of HCl.
The front end of quartz ampoule 1 is connected by connecting tube with HCl steel cylinder 5, and regulating valve 6 and flow are serially connected in the connecting tube
Table 7.
The discharge end of quartz ampoule 1 connects Guan Cha bottle 3 by pipeline, and the upper end of Guan Cha bottle 3 connects spray equipment by pipeline
4。
Three layers of filler layer 14 placed separately is provided in spray equipment 4.
It is equipped with lye 15 and lye 16 respectively in Guan Cha bottle 3 and spray equipment 4 when production, on three layers of filler layer 14 placed separately
Filler is launched respectively --- polyhedron empty ball plastic sphere.Tail gas containing HCl carries out gas-liquid two-phase with lye absorbing liquid and comes into full contact with
Neutralization reaction is absorbed, tail gas is discharged into atmosphere after purification.Lye absorbing liquid tower bottom after water pump is pressurized tower top spray and
Under, finally it is back to tower bottom recycling.
Outside spray equipment 4 arrange NaOH solution circulating pump 13, the liquid outlet and inlet of NaOH solution circulating pump 13 respectively with spray
The top and bottom of device 4 are connected.
Four fluorine tube can be used in above each pipeline, to prevent metal impurities element pollution.
Two, process example:
Embodiment 1:
It will be loaded into silica crucible containing miscellaneous high-purity silicon carbide material by with a thickness of 3cm, then silica crucible be placed in quartz ampoule
It is interior (as shown in Figure 1), the heating element of heating jacket 8 is opened, makes to rise to 1200 DEG C containing miscellaneous high-purity silicon carbide temperature of charge, so
It is passed through high-purity HCl gas that flow is 2L/min afterwards, reaction carries out under 3~5mmHg pressure condition, stops after 2 hours logical
Enter HCl gas, after cooling, opens quartz ampoule, unreacted solid is collected from silica crucible.
The above unreacted solid is carried out to carry out Element detection through ICP-MS to get impurity element in the product after removal of impurities
Content is respectively as follows: boron≤0.2ppm, aluminium≤0.3ppm, titanium≤0.3ppm, iron≤0.2ppm, and vanadium≤0.2ppm reaches 5~6N's
Purity requirement.
And it is respectively as follows: boron≤0.5ppm containing miscellaneous high-purity silicon carbide material impurity content before not being passed through HCl, aluminium≤0.6ppm,
Titanium≤0.8ppm, iron≤1ppm, vanadium≤0.5ppm.
Embodiment 2:
The device of reference example 1 by high-purity silicon carbide material by being filled with a thickness of 4cm after, then will be containing miscellaneous high-purity silicon carbide material
Temperature rises to 900 DEG C, is passed through high-purity 5L/minHCl gas, and reaction carries out under 3~5mmHg pressure condition, and time 2 h is anti-
It should terminate.
Product after removal of impurities carries out Element detection, impurity content through ICP-MS are as follows: boron≤0.2ppm, aluminium≤
0.4ppm, titanium≤0.3ppm, iron≤0.3ppm, vanadium≤0.2ppm reach the purity requirement of 5~6N.
And it is not passed through impurity before HCl are as follows: boron≤0.5ppm, aluminium≤0.6ppm, titanium≤0.8ppm, iron≤1ppm, vanadium≤
0.5ppm。
Embodiment 3:
The device of reference example 1 by high-purity silicon carbide material by being filled with a thickness of 5cm after, then will be containing miscellaneous high-purity silicon carbide material
Temperature rises to 900 DEG C, is passed through high-purity 2L/minHCl gas, and reaction carries out under 3~5mmHg pressure condition, and the reaction time 4 is small
When.
Product after removal of impurities carries out Element detection, impurity content through ICP-MS are as follows: boron≤0.1ppm, aluminium≤
0.2ppm, titanium≤0.3ppm, iron≤0.3ppm, vanadium≤0.1ppm reach the purity requirement of 5~6N.
And it is not passed through impurity before HCl are as follows: boron≤0.5ppm, aluminium≤0.6ppm, titanium≤0.8ppm, iron≤1ppm, vanadium≤
0.5ppm。
Embodiment 4:
The device of reference example 1 by high-purity silicon carbide material by being filled with a thickness of 2cm after, then will be containing miscellaneous high-purity silicon carbide material
Temperature rises to 900 DEG C, is passed through high-purity 2L/minHCl gas, and reaction carries out under 3~5mmHg pressure condition, and the reaction time 4 is small
When.
Product after removal of impurities carries out Element detection through ICP-MS, and impurity content is boron≤0.1ppm, aluminium≤0.2ppm,
Titanium≤0.2ppm, iron≤0.2ppm, vanadium≤0.1ppm reach the purity requirement of 5~6N.
And not being passed through impurity before HCl is boron≤0.5ppm, aluminium≤0.6ppm, titanium≤0.8ppm, iron≤1ppm, vanadium≤
0.5ppm。
Embodiment 5:
The device of reference example 1 by high-purity silicon carbide material by being filled with a thickness of 1cm after, then will be containing miscellaneous high-purity silicon carbide material
Temperature rises to 900 DEG C, is passed through high-purity 2L/minHCl gas, and reaction carries out under 3~5mmHg pressure condition, and the reaction time 4 is small
When.
Product after removal of impurities carries out Element detection through ICP-MS, and impurity content is boron≤0.1ppm, aluminium≤0.3ppm,
Titanium≤0.2ppm, iron≤0.2ppm, vanadium≤0.1ppm reach the purity requirement of 5~6N.
And it is not passed through impurity before HCl are as follows: boron≤0.5ppm, aluminium≤0.6ppm, titanium≤0.8ppm, iron≤1ppm, vanadium≤
0.5ppm。
Claims (10)
1. the method that depth removes impurity element in high-purity silicon carbide powder, it is characterised in that be passed through temperature with HCl gas as 900
~1200 DEG C contain miscellaneous silicon carbide powder, make to react the low-boiling chlorine of generation with HCl containing the impurity element in miscellaneous silicon carbide powder
The low-boiling chloride of generation is discharged compound, collects unreacted solid, i.e. the purity silicon carbide powder that is 5~6N.
2. according to the method described in claim 1, it is characterized in that by containing miscellaneous silicon carbide powder be loaded into silica crucible into
Row reaction.
3. according to the method described in claim 2, it is characterized in that when loading the silicon carbide materials with a thickness of 1~5cm.
4. according to the method described in claim 3, it is characterized in that when loading the silicon carbide materials with a thickness of 2cm.
5. the method according to claim 3 or 4, it is characterised in that the HCl gas flow is 2~5L/min.
6. according to the method described in claim 1, it is characterized in that the reaction carries out under 3~5mmHg pressure condition.
7. method according to claim 1 or 6, it is characterised in that the reaction time is 2~4 hours.
8. according to the method described in claim 1, it is characterized in that the low-boiling chloride of generation is absorbed in lye.
9. according to the method described in claim 2, it is characterized in that the silica crucible is placed in quartz ampoule.
10. according to the method described in claim 9, it is characterized in that quartz is arranged in the silica crucible periphery in the quartz ampoule
The flow plug of material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114113039A (en) * | 2021-11-23 | 2022-03-01 | 株洲科能新材料股份有限公司 | Detection method and detection device for high purity carbon |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555010A (en) * | 2008-04-12 | 2009-10-14 | 于旭宏 | Carborundum |
| CN102432011A (en) * | 2011-10-08 | 2012-05-02 | 江苏佳宇资源利用股份有限公司 | Method for synchronously removing iron and silicon impurities in silicon carbide micro-powder |
| CN103241742A (en) * | 2013-05-13 | 2013-08-14 | 杨恺 | High-purity SiCl4 purification method |
| CN109160511A (en) * | 2018-09-17 | 2019-01-08 | 厦门大学 | A kind of device and method of graphite purification |
-
2019
- 2019-02-28 CN CN201910152688.8A patent/CN109721056A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555010A (en) * | 2008-04-12 | 2009-10-14 | 于旭宏 | Carborundum |
| CN102432011A (en) * | 2011-10-08 | 2012-05-02 | 江苏佳宇资源利用股份有限公司 | Method for synchronously removing iron and silicon impurities in silicon carbide micro-powder |
| CN103241742A (en) * | 2013-05-13 | 2013-08-14 | 杨恺 | High-purity SiCl4 purification method |
| CN109160511A (en) * | 2018-09-17 | 2019-01-08 | 厦门大学 | A kind of device and method of graphite purification |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114113039A (en) * | 2021-11-23 | 2022-03-01 | 株洲科能新材料股份有限公司 | Detection method and detection device for high purity carbon |
| CN114113039B (en) * | 2021-11-23 | 2023-09-26 | 株洲科能新材料股份有限公司 | Method and device for detecting purity of high-purity carbon |
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Application publication date: 20190507 |