CN208700586U - The preparation facilities of disilane - Google Patents
The preparation facilities of disilane Download PDFInfo
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- CN208700586U CN208700586U CN201821282840.1U CN201821282840U CN208700586U CN 208700586 U CN208700586 U CN 208700586U CN 201821282840 U CN201821282840 U CN 201821282840U CN 208700586 U CN208700586 U CN 208700586U
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Abstract
One embodiment of the utility model provides a kind of preparation facilities of disilane, including filter element, first rectifying column, Second distillation column and reactor；Wherein, the first rectifying column is connected with the filter element, and the Second distillation column is connected with the first rectifying column, and the reactor is connected with the Second distillation column.The device of one embodiment of the utility model can prepare the high-purity disilane for meeting semicon industry application using polysilicon raffinate as raw material.
Description
Technical field
The utility model relates to the preparation facilities of disilane, specially a kind of to prepare the height for meeting semicon industry application
The preparation facilities of pure disilane.
Background technique
Disilane is mainly used for the side such as solar battery, photosensitive rotating cylinder, amorphous silicon film, epitaxial growth, chemical vapor deposition
Face.When as sedimentary origin, sedimentary is silicon oxide or silicon nitride, compared with silane, disilane have deposition velocity faster, deposition
The lower feature of temperature can prevent from generating ball bumps in unformed silicon, can be improved the homogeneity being deposited into, be mainly used in
The manufacture of 20 nanometers or less high-end chips.
It is more faster in the deposition velocity of amorphous silicon on piece than with silane with disilane in manufacture of solar cells, and temperature
Degree can reduce by 200~300 DEG C；In ion implanting, make that Yi Qihui after ion source, line are strong, and effect is significantly better than with disilane
Make ion source with other gases；It is used for extension and diffusion technique in semiconductor processing, is also used for solar battery and electronics shines
Photosensitive drums mutually；When using disilane, expensive quartz glass can be replaced to make the base of LCD using the lower glass of price
Material.
Currently, the preparation of disilane mainly has chloro disilane reduction method and magnesium silicide to react two kinds of sides of synthesis with ammonium chloride
Method.Wherein, chloro disilane reduction method is the complex metal hydrides deoxygenization chlorination disilane alkane such as lithium aluminium hydride reduction or sodium aluminum hydride
Disilane is prepared, but in this method, chloro disilane needs to carry out separately synthesized, and synthesis difficulty is big and low yield.
And magnesium silicide is that magnesium silicide carries out reacting generation disilane with ammonium chloride, but produces in the process with ammonium chloride reaction method
Product are mainly silane, and disilane accounting is to be recycled as by-product, therefore main pass through controls pair only 3% or so
The yield of product improves disilane yield, limits the feasibility that this method produces disilane as major product.
Utility model content
One main purpose of the utility model is providing a kind of preparation facilities of disilane, including filter element, first
Rectifying column, Second distillation column and reactor；Wherein, the first rectifying column is connected with the filter element, second rectifying
Tower is connected with the first rectifying column, and the reactor is connected with the Second distillation column.
According to one embodiment of the utility model, the filter element includes one or more filters.
According to one embodiment of the utility model, the reactor is micro passage reaction.
According to one embodiment of the utility model, the first rectifying column is connected by tower top with the Second distillation column,
The Second distillation column is connected by tower reactor with the reactor.
It further include the third distillation column being sequentially connected, the 4th rectifying column and the 5th according to one embodiment of the utility model
Rectifying column, the third distillation column are connected with the reactor.
According to one embodiment of the utility model, the reactor is connected by top with the third distillation column, described
Third distillation column is connected by tower top with the 4th rectifying column, and the 4th rectifying column passes through tower reactor and the 5th rectifying column
It is connected.
It further include impurity collector according to one embodiment of the utility model, the impurity collector is respectively with described
The tower reactor of one rectifying column, the tower top of the Second distillation column, the tower reactor of the third distillation column, the 4th rectifying column tower top
And the tower top of the 5th rectifying column is connected.
It further include the absorbing unit being connected with the 5th rectifying column according to one embodiment of the utility model.
According to one embodiment of the utility model, the 5th rectifying column is connected by tower reactor with the absorbing unit
According to one embodiment of the utility model, the absorbing unit includes one or more absorbers.
The device of one embodiment of the utility model can be prepared using polysilicon raffinate as raw material and meet semicon industry
The high-purity disilane of application.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the preparation facilities of the disilane of one embodiment of the utility model；
Fig. 2 is the flow chart for preparing disilane of one embodiment of the utility model.
Specific embodiment
The exemplary embodiment for embodying the utility model features and advantages will describe in detail in the following description.It should be understood that
Be that the utility model can have various variations in different embodiments, all do not depart from the model of the utility model
It encloses, and the descriptions and illustrations are essentially for illustration purposes, rather than to limit the utility model.
In improved Siemens polysilicon production process, a small amount of chloro second silicon can be generated in reduction process and hydrogenation process
Alkane, chloro disilane are a silicon hexachloride, two silicon hexachlorides, trichloroethyl silane, four silicon hexachlorides, five silicon hexachlorides and hexachloroethanc
The mixture of silane, above-mentioned chloro disilane is enriched in polysilicon raffinate after concentration.
One embodiment of the utility model provides a kind of preparation facilities of disilane, and can be used for will be in polysilicon raffinate
Chloro disilane is recycled and is refined, and prepares disilane by reduction reaction.
As shown in Figure 1, the preparation facilities of the disilane of one embodiment of the utility model, including the filtering list being sequentially communicated
Member 10, first rectifying column 21, Second distillation column 22 and reactor 30.
In conjunction with Fig. 2, can by filter element 10, first rectifying column 21, Second distillation column 22 to raw material polysilicon raffinate into
Row filtering, rectification process, obtain the chloro disilane of high-purity, and chloro disilane can carry out reduction reaction in reactor 30,
Generate disilane.
Polysilicon raffinate is filtered by filter element 10, can remove solid impurity, the solid impurity for example comprising
Particulate material, metal-containing polymer, impurity containing amorphous silicon and metal etc..
In an embodiment, the removal rate of solid impurity in filter element 10, mistake can be controlled by adjusting filtering accuracy
Filtering precision is preferably 0.5~1 μm.Filtering accuracy control can be removed farthest within the above range containing amorphous silicon and
The impurity of metal, filtering accuracy is too small, and filter is easy blocking to frequently overhaul, and the excessive then removal rate of filtering accuracy reduces.
In an embodiment, filter element 10 includes the filter of one or more serial or parallel connection operation.In part
When filter overhauls, come into operation shunt filter, it is ensured that system continuous operation.
In an embodiment, the filter of filter element 10 is accurate filter, and accurate filter includes shell and sets
Floral disc and filter core inside housings is set, filter core is mounted on floral disc.
In an embodiment, filter core is more, and the particular number of filter core can be determined according to filtration treatment amount.
In an embodiment, filter core is metal filtering core, ceramic element or polytetrafluoroethylene (PTFE) filter core.
In an embodiment, first rectifying column 21 is connected by tower top with Second distillation column 22, Second distillation column 22
It is connected by tower reactor with reactor 30.
In an embodiment, preparation facilities further includes impurity collector 40, respectively with the tower reactor of first rectifying column 21,
The tower top of Second distillation column 22 is connected.
In an embodiment, reactor 30 can be micro passage reaction, and reactor material is metal, glass, carbonization
The materials such as silicon, inside reactor channel diameter are 0.5~10 micron, by reducing reaction channel, improve the mass tranfer coefficient of reaction.
In an embodiment, reactor 30 can be the reactor with temperature control, pressure control and agitating function, and material can be with
For 316L stainless steel, internal electrobrightening.
In an embodiment, multiple impellers, stirring variable speed etc. is can be used in the whipped form of reactor 30.
In an embodiment, reactor 30 includes reaction inner cavity, vacuum jacket, agitating device and feeding device.Reaction
Inner cavity can be cylindrical housings, and volume can be 0.5~5m3, preferably 3m3, wall thickness is 4~8mm, and pressure is 3~4bar.Very
Empty collet is set to the outside of reaction inner cavity, can be set -30 DEG C of glycol-cooled media in collet, and collet volume is 0.1~
0.5m3, pressure is 2~10Pa, is equipped with feed opening in reactor head, each material can pass through respectively feed opening by control system
Reactor 30 is added.
In an embodiment, preparation facilities further includes the third distillation column 23 being sequentially connected, the 4th rectifying column 24 and
Five rectifying columns 25, third distillation column 23 are connected with reactor 30.Pass through third distillation column 23, the 4th rectifying column 24 and the 5th essence
It evaporates 25 pairs of reaction products therefroms of tower and carries out rectifying purification process, the high-purity disilane for meeting semicon industry application can be obtained.
Wherein, reactor 30 is connected by its top with third distillation column 23, and third distillation column 23 passes through tower top and the
Four rectifying columns 24 are connected, and the 4th rectifying column 24 is connected by tower reactor with the 5th rectifying column 25.
In an embodiment, the tower top and the 5th rectifying column 25 of the tower reactor of third distillation column 23, the 4th rectifying column 24
Tower top be connected respectively with impurity collector 40.
It further include the absorbing unit being connected with the tower reactor of the 5th rectifying column 25 in an embodiment.By using rectifying
Joint adsorption may be implemented that disilane product is further purified, promote the quality of product.
In an embodiment, for the continuous operation for guaranteeing adsorption effect and system, absorbing unit may include one or more
A absorber, the filler in absorber can be molecular sieve and/or active carbon.
In an embodiment, absorbing unit includes the absorber 31 and absorber 32 being sequentially connected, absorber 31 and
The tower reactor of five rectifying columns 25 is connected, and active carbon can be arranged in absorber 31, molecular sieve is arranged in absorber 32.Through adsorbing
After the adsorption treatment of device 31 and absorber 32, the disilane of purity 5N can be obtained.
Hereinafter, the work flow in conjunction with Fig. 1, the preparation facilities of the disilane of 2 pairs of one embodiments of the utility model carries out
It further illustrates.
After the filtering of filter element 10, resulting filtrate enters first rectifying column 21 and carries out at the first rectifying polysilicon raffinate
Reason, to remove the high-boiling-point impurity in filtrate, which includes high-boiling components and metal polymer in polysilicon raffinate.
Filtrate is separated into overhead vapours and tower reactor Liquid Residue through the processing of first rectifying column 21, and the high-boiling-point impurities such as high-boiling components stay in
The tower reactor of one rectifying column 21, and enter impurity collector 40, the steam comprising chloro disilane is discharged from tower top, obtains after condensation
First tower top rectifying liquid.
Wherein, the tower top pressure of first rectifying column 21 can be 50~120KPa, such as 70KPa, 90KPa, 110KPa
Deng；The tower top temperature of first rectifying column 21 can be 90~130 DEG C, such as 100 DEG C, 110 DEG C, 120 DEG C etc.；First rectifying column
21 plate theory series can be 60~120, such as 70,90,100,110 etc..
Later, the first tower top rectifying liquid enters the second rectification process of progress of Second distillation column 22, includes trichlorine hydrogen to remove
The low-boiling-point substances impurity such as silicon, silicon tetrachloride.After the processing of Second distillation column 22, low-boiling-point substance is discharged into impurity collector from tower top
40, tower reactor collects high-purity chloro for disilane.
The tower top pressure of Second distillation column 22 can be 40~100KPa, such as 50KPa, 70KPa, 90KPa etc.；Second
The tower top temperature of rectifying column 22 can be 90~110 DEG C, such as 95 DEG C, 100 DEG C, 105 DEG C etc.；The column plate of Second distillation column 22
Theoretical stage can be 70~90, such as 75,80,85 etc..
The high-purity chloro collected from 22 tower reactor of Second distillation column enters reactor 30 and complex metal hydride for disilane
(such as lithium aluminium hydride reduction, sodium aluminum hydride, diethylaluminum hydride) reacts, and generates disilane.Specific reaction equation for example may is that
LiAlH4+Si2HmCln—Si2H6+LiCl+AlCl3(m+n=6)
Wherein, reaction can carry out in ether and/or tetrahydrofuran solvent, and by-product silicon has been supervened in reaction process
Alkane.
It is discharged at the top of reacting rear material autoreactor 30, carries out third rectification process into third distillation column 23, to remove
Remaining reaction dissolvent, chloro disilane etc..After the processing of third distillation column 23, remaining reaction dissolvent, chloro disilane etc.
It is discharged into impurity collector 40 from tower reactor, overhead extraction includes the material of disilane.Wherein, third distillation column is weight-removing column,
Tower top temperature is -10~10 DEG C.
Material comprising disilane enters the 4th rectifying column 24 and carries out the 4th rectification process, with remove boiling point lower than -50~-
The low-boiling by-products such as 30 DEG C of silane, hydrogen, hydrogen chloride, the tower top temperature of the 4th rectifying column 24 of control are -50~-30 DEG C,
Low-boiling products of the boiling point lower than -50~-30 DEG C are discharged into impurity collector 40 from tower top, and tower reactor produces material and enters the 5th
Rectifying column 25.
Material carries out the 5th rectification process in the 5th rectifying column 25, to remove the chloro second silicon that boiling point is lower than -20~-15 DEG C
The low-boiling by-products such as alkane, silane, hydrogen chloride.Controlling 25 tower top temperature of the 5th rectifying column is -20~-15 DEG C, and boiling point is lower than -20
~-15 DEG C of low-boiling products are discharged into impurity collector 40, tower reactor output 4N disilane from tower top.
For the purity for further increasing disilane product, the disilane that the 5th rectifying column 25 is discharged can be sequentially sent into filling
The absorber 31 of active charcoal and the absorber 32 for being filled with molecular sieve carry out adsorption and purification processing, obtain 5N disilane.
Using polysilicon raffinate as raw material, it can be prepared by the device of one embodiment of the utility model and meet semiconductor row
The high-purity disilane of industry application.
Unless limited otherwise, term used in the utility model is the normally understood meaning of those skilled in the art.
Embodiment described in the utility model is merely for exemplary purpose, not to limit the guarantor of the utility model
Range is protected, those skilled in the art can make various other replacements, changes and improvements in the scope of the utility model, thus,
The present invention is not limited to the above embodiments, and is only defined by the claims.
Claims (10)
1. a kind of preparation facilities of disilane characterized by comprising
Filter element；
First rectifying column is connected with the filter element；
Second distillation column is connected with the first rectifying column；And
Reactor is connected with the Second distillation column.
2. the apparatus according to claim 1, which is characterized in that the filter element includes one or more filters.
3. the apparatus according to claim 1, which is characterized in that the reactor is micro passage reaction.
4. the apparatus according to claim 1, which is characterized in that the first rectifying column passes through tower top and second rectifying
Tower is connected, and the Second distillation column is connected by tower reactor with the reactor.
5. the apparatus according to claim 1, which is characterized in that further include the third distillation column being sequentially connected, the 4th rectifying
Tower and the 5th rectifying column, the third distillation column are connected with the reactor.
6. device according to claim 5, which is characterized in that the reactor passes through top and the third distillation column phase
Even, the third distillation column is connected by tower top with the 4th rectifying column, and the 4th rectifying column passes through tower reactor and described the
Five rectifying columns are connected.
7. device according to claim 5, which is characterized in that it further include impurity collector, the impurity collector difference
With the tower reactor of the first rectifying column, the tower top of the Second distillation column, the tower reactor of the third distillation column, the 4th rectifying
The tower top of the tower top of tower and the 5th rectifying column is connected.
8. device according to claim 5, which is characterized in that further include the absorption list being connected with the 5th rectifying column
Member.
9. device according to claim 8, which is characterized in that the 5th rectifying column passes through tower reactor and the absorbing unit
It is connected.
10. device according to claim 8, which is characterized in that the absorbing unit includes one or more absorbers.
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| CN201821282840.1U CN208700586U (en) | 2018-08-09 | 2018-08-09 | The preparation facilities of disilane |
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| CN201821282840.1U CN208700586U (en) | 2018-08-09 | 2018-08-09 | The preparation facilities of disilane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108751201A (en) * | 2018-08-09 | 2018-11-06 | 洛阳中硅高科技有限公司 | The preparation facilities of disilane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108751201A (en) * | 2018-08-09 | 2018-11-06 | 洛阳中硅高科技有限公司 | The preparation facilities of disilane |
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