CN104362114B - A kind of large diameter zone melting cleaning device and its cleaning method of polycrystalline bar - Google Patents
A kind of large diameter zone melting cleaning device and its cleaning method of polycrystalline bar Download PDFInfo
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- CN104362114B CN104362114B CN201410525225.9A CN201410525225A CN104362114B CN 104362114 B CN104362114 B CN 104362114B CN 201410525225 A CN201410525225 A CN 201410525225A CN 104362114 B CN104362114 B CN 104362114B
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- acid
- polycrystalline
- polycrystalline bar
- large diameter
- zone melting
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- 238000004140 cleaning Methods 0.000 title claims abstract description 47
- 238000004857 zone melting Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 71
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 52
- 230000007797 corrosion Effects 0.000 claims abstract description 44
- 238000005260 corrosion Methods 0.000 claims abstract description 44
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 19
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 238000005554 pickling Methods 0.000 claims description 6
- 238000005096 rolling process Methods 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 4
- 235000011194 food seasoning agent Nutrition 0.000 claims description 4
- 238000006396 nitration reaction Methods 0.000 claims description 4
- 238000010301 surface-oxidation reaction Methods 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052710 silicon Inorganic materials 0.000 abstract description 6
- 239000010703 silicon Substances 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 229960002050 hydrofluoric acid Drugs 0.000 description 9
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 229920005591 polysilicon Polymers 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229940023184 after bite Drugs 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
Abstract
The invention provides a kind of cleaning device of large diameter zone melting with polycrystalline bar; belong to semi-conducting material cleaning technique field; including operating room, feeding platform and blanking bench; precleaning unit, acid corrosion groove, ultrasonic cleaning equipment and drying unit are disposed between feeding platform and blanking bench; slid back and forth at the top of operating room and be connected with two material transferring devices, a QRD nitrogen protection devices are additionally provided between acid corrosion groove and ultrasonic cleaning equipment.The invention also discloses a kind of cleaning method of large diameter zone melting with polycrystalline bar.The present invention can complete the automatic cleaning process of the 160mm polycrystalline bars of diameter 140, save manpower, stabilize the quality after product is washed；Suitable for removal of the large diameter zone melting with the metal impurities of polycrystalline billet surface, make polycrystalline bar surface no-pollution, improve policrystalline silicon quality and crystal forming rate.
Description
Technical field
The present invention relates to belong to semi-conducting material cleaning technique field, specifically a kind of large diameter zone melting polycrystalline bar
Cleaning device and its cleaning method.
Background technology
At present, the method that the impurity level on the surface of block or rod-like polycrystal silicon is generally cleaned using reagent, for except impurity elimination
The reagent of matter has：The mixture of hydrogen fluorine/hydrogen peroxide aqueous acid and water, pure water, mixed liquor of nitric acid and hydrofluoric acid etc., use this
A little reagents clean the surface of polysilicon.Prior art is the mixed acid solution using nitric acid and hydrofluoric acid, and policrystalline silicon surface is carried out
Corrosion, is then rinsed to polycrystalline bar using deionized water, dried, cooling packing.This process carries out polycrystalline by manpower
The processing cleaning of bar, inefficiency, cleaning quality is not sufficiently stable.
The content of the invention
The problem to be solved in the present invention is：The deficiencies in the prior art are overcome to remove large diameter zone melting polycrystalline there is provided one kind
The metal impurities of billet surface, make polycrystalline bar surface no-pollution, improve policrystalline silicon quality, improve crystal forming rate, automaticity
Height, labor intensity is small, the sour harm to the human body small large diameter zone melting cleaning device of polycrystalline bar.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of large diameter zone melting polycrystalline bar
Cleaning device, including operating room and be arranged on the feeding platform and blanking bench of operating room front and back ends, the feeding platform and blanking bench it
Between be disposed with precleaning unit, acid corrosion groove, ultrasonic cleaning equipment and drying unit, the precleaning unit and sour
Erosion device is rolling cleaning, and the precleaning unit is a tank, and the bottom of the tank is provided with several roller bearings, the water
The top inward flange of groove, which is provided with to slide back and forth at the top of high-pressure water nozzle, the operating room, is connected with two material transferring devices,
One of material transferring device be located between feeding platform and acid corrosion groove, another material transferring device be located at acid corrosion groove and
Between blanking bench, a QDR nitrogen protection devices, the QDR are additionally provided between the acid corrosion groove and ultrasonic cleaning equipment
Nitrogen protection device is several nitrogen sprayer heads, and the nitrogen sprayer head is arranged between acid corrosion groove and ultrasonic cleaning equipment.
Further, the bottom of the acid corrosion groove is made up of row's roller bearing.
Further, the material of the acid corrosion groove is PT or PVC materials.
Further, an automatic acid adder is connected on the side wall of the acid corrosion groove, the automatic acid adder can be right
Mixed acid solution in acid corrosion groove is fed and replaced.
Further, the rear end of the operating room provided with a wind drench window, the blanking bench be located at wind drench window just under
Side.
The invention solves the problems that another problem be：A kind of automatic flushing device of large diameter zone melting polycrystalline bar is provided
Cleaning method.
A kind of large diameter zone melting cleaning method of the cleaning device of polycrystalline bar, comprises the following steps：
(1) feeding：Polycrystalline bar is positioned over feeding platform, prerinse is then carried out；
(2) prerinse：The surface blot of polycrystalline bar is cleaned；
(3) pickling：By polycrystalline bar be put into acid solution in rotary rolling in acid corrosion groove, the acid corrosion groove for nitric acid with
The mixed acid solution of hydrofluoric acid；
(4) QDR nitrogen sparges：After pickling terminates, the polycrystalline bar in acid corrosion groove is taken out and is put into ultrasonic sink
In, this process needs to use nitrogen sparge to protect, and prevents polycrystalline bar surface oxidation；
(5) it is ultrasonic：By vibration of ultrasonic wave, the acid solution and impurity of polycrystalline billet surface are removed；
(6) dry：Hot-air seasoning polycrystalline bar；
(7) blanking：Polycrystalline bar is placed on blanking bench after wind drenches window.
Further, the proportioning of the nitration mixture is that the volume ratio of nitric acid and hydrofluoric acid is 7.5：1.
Further, a length of 3min during the nitrogen sparge.
Further, a length of 15min when described ultrasonic.
Further, the drying temperature is 60-90 DEG C, and drying time is 10-15min.
The present invention has the advantages and positive effects of：
Using the automatic cleaning equipment of polycrystalline bar, the automatic of diameter 140-160mm polycrystalline bars can be completed and cleaned
Journey, saves manpower, stabilizes the quality after product is washed；The present invention is suitable for metal of the large diameter zone melting with polycrystalline billet surface
The removal of impurity, makes polycrystalline bar surface no-pollution, improves policrystalline silicon quality, improves crystal forming rate.
Brief description of the drawings
Fig. 1 is the front view of the cleaning device of large diameter zone melting polycrystalline bar of the present invention.
Fig. 2 is the top view of the cleaning device of large diameter zone melting polycrystalline bar of the present invention.
In figure：1st, operating room；2nd, feeding platform；3rd, blanking bench；4th, precleaning unit；5th, acid corrosion groove；6th, ultrasonic wave is cleaned
Device；7th, drying unit；8th, material transferring device；9th, QRD nitrogen protection devices；10th, automatic acid adder；11st, wind drenches window.
Embodiment
As shown in Figure 1 and Figure 2, a kind of large diameter zone melting cleaning device of polycrystalline bar, including operating room 1 and be arranged on
The feeding platform 2 and blanking bench 3 of the front and back ends of operating room 1, are disposed with precleaning unit 4, acid between feeding platform 2 and blanking bench 3
Etching tank 5, ultrasonic cleaning equipment 6 and drying unit 7.Precleaning unit 4 is a tank, and the bottom of tank is rolled provided with several
Axle, the top edge of tank is provided with high-pressure water nozzle, and prerinse is carried out to polycrystalline bar.The bottom of PVC acid corrosion device 5 is
It is made up of row's PVC roller bearings, can prevents from connecting an automatic acid adder 10 on the corrosion of strong acid, the side wall of acid corrosion groove 5,
Automatic acid adder 10 can mix nitric acid with hydrofluoric acid proportioning, and then the mixed acid solution in acid corrosion groove 5 is fed
And replacement.The top of operating room 1, which slides back and forth, is connected with two material transferring devices 8, and one of material transferring device is located at
Between feeding platform 2 and acid corrosion groove 5, another material transferring device is located between acid corrosion groove 5 and blanking bench 3, material transfer
Device 8 is mechanical arm, and polycrystalline bar can be transferred to latter arrangement by mechanical arm by previous device.Acid corrosion groove 5 and ultrasonic wave are clear
A QRD nitrogen protection devices 9 are additionally provided between cleaning device 6, QRD nitrogen protection devices 9 are several nitrogen sprayer heads, nitrogen spray
Head is arranged between acid corrosion groove 5 and ultrasonic cleaning equipment 6, to being shifted between acid corrosion groove 5 and ultrasonic cleaning equipment 6
Polycrystalline rod carry out nitrogen sparge protection, prevent polycrystalline bar surface oxidation.Drying unit 7 is air flow dryer, operating room 1
Rear end provided with a wind drench window 11, blanking bench 3 be located at wind drench window 11 just under.
A kind of large diameter zone melting cleaning method of the cleaning device of polycrystalline bar, comprises the following steps：
(1) feeding：Polycrystalline bar is positioned over feeding platform 1, prerinse is then carried out；
(2) prerinse：The surface blot of polycrystalline bar is cleaned；
(3) pickling：Acid solution polycrystalline bar being put into rotary rolling in acid corrosion groove 5, acid corrosion groove 5 is nitric acid and hydrogen
The mixed acid solution of fluoric acid, the proportioning of nitration mixture is that the volume ratio of nitric acid and hydrofluoric acid is 7.5：1.
(4) QDR nitrogen sparges：After pickling terminates, the polycrystalline bar in acid corrosion groove is taken out and is put into ultrasonic sink
In, this process needs to use nitrogen sparge to protect, and prevents polycrystalline bar surface oxidation, a length of 3min during nitrogen sparge.
(5) it is ultrasonic：By vibration of ultrasonic wave, a length of 15min when ultrasonic removes the acid solution and impurity of polycrystalline billet surface；
(6) dry：Hot-air seasoning polycrystalline bar, drying temperature is 60-90 DEG C, and drying time is 10-15min；
(7) blanking：Polycrystalline bar is drenched after window wind drenches by wind and is placed on blanking bench.
The course of work of this example：Polycrystalline bar is placed on feeding platform 1, polycrystalline bar is put into pre- by mechanical arm automatically
In the tank of cleaning device 4, the roller of bottom of gullet, which is rotated, drives polycrystalline rod material to rotate, the high pressure water jets of the top edge of tank
Head is sprayed polycrystalline bar, completes the cleaning of the silica flour and greasy dirt of polysilicon billet surface.After prerinse is finished, machinery
Arm takes out the polycrystalline bar in tank, is slowly put into acid corrosion groove 5, and the proportioning of nitration mixture is the volume ratio of nitric acid and hydrofluoric acid
For 7.5：1, the automatic rotary rolling corrosion in acid corrosion groove 5 of polycrystalline bar.After bite terminates, mechanical arm is by acid corrosion groove
Polycrystalline bar in 5 takes out, and nitrogen sprayer head carries out nitrogen sparge 3min to polycrystalline rod, is then transferred to ultrasonic cleaning equipment 6
In, ultrasonic vibration 15min, by the acid solution and Impurity removal of polycrystalline billet surface.After ultrasonic cleaning is finished, mechanical arm is by polycrystalline rod
Material is moved in drying unit 7, in 60-90 DEG C of hot-air seasoning 10-15min.Mechanical arm drenches the polycrystalline bar after drying by wind
After the wind of window 11 drenches, it is placed on blanking bench 3, the cleaning of polycrystalline bar is completed.With the growth of acid corrosion time, mixed acid is molten
The concentration of liquid changes, and automatic acid adder 10 can mix nitric acid with hydrofluoric acid proportioning, then to the acid in acid corrosion groove 5
Fed and replaced.
Using the automatic cleaning equipment of polycrystalline bar, the automatic of diameter 140-160mm polycrystalline bars can be completed and cleaned
Journey, saves manpower, stabilizes the quality after product is washed；The present invention is suitable for metal of the large diameter zone melting with polycrystalline billet surface
The removal of impurity, makes polycrystalline bar surface no-pollution, improves policrystalline silicon quality, improves crystal forming rate.
One embodiment of the present of invention is described in detail above, but the content is only the preferable reality of the present invention
Example, it is impossible to be considered as the practical range for limiting the present invention.All impartial changes made according to the present patent application scope and improvement
Deng within the patent covering scope that all should still belong to the present invention.
Claims (10)
1. a kind of large diameter zone melting cleaning device of polycrystalline bar, including operating room and it is arranged on the upper of operating room front and back ends
Expect platform and blanking bench, it is characterised in that：Be disposed between the feeding platform and blanking bench precleaning unit, acid corrosion groove,
Ultrasonic cleaning equipment and drying unit, the precleaning unit and acid corrosion device are rolling cleaning, the prerinse dress
A tank is set to, the bottom of the tank is provided with several roller bearings, and the top inward flange of the tank is provided with high-pressure water nozzle, institute
To state slide back and forth at the top of operating room and be connected with two material transferring devices, one of material transferring device be located at feeding platform and
Between acid corrosion groove, another material transferring device is located between acid corrosion groove and blanking bench, the acid corrosion groove and ultrasonic wave
A QDR nitrogen protection devices are additionally provided between cleaning device, the QDR nitrogen protection devices are several nitrogen sprayer heads, institute
Nitrogen sprayer head is stated to be arranged between acid corrosion groove and ultrasonic cleaning equipment.
2. a kind of large diameter zone melting according to claim 1 cleaning device of polycrystalline bar, it is characterised in that：The acid
The bottom of etching tank is made up of row's roller bearing.
3. a kind of large diameter zone melting according to claim 2 cleaning device of polycrystalline bar, it is characterised in that：The acid
The material of etching tank is PT or PVC materials.
4. a kind of large diameter zone melting according to claim 1 cleaning device of polycrystalline bar, it is characterised in that：The acid
An automatic acid adder is connected on the side wall of etching tank, the automatic acid adder can enter to the mixed acid solution in acid corrosion groove
Row supply and replacement.
5. a kind of large diameter zone melting according to claim 1 cleaning device of polycrystalline bar, it is characterised in that：The behaviour
Window is drenched in the rear end for making room provided with a wind, and the blanking bench is located at the underface that wind drenches window.
6. a kind of large diameter zone melting as claimed in claim 1 cleaning method of the cleaning device of polycrystalline bar, its feature exists
In：Comprise the following steps：
(1) feeding：Polycrystalline bar is positioned over feeding platform, prerinse is then carried out；
(2) prerinse：The surface blot of polycrystalline bar is cleaned；
(3) pickling：It is nitric acid and hydrogen fluorine that polycrystalline bar is put into the acid solution in rotary rolling in acid corrosion groove, the acid corrosion groove
The mixed acid solution of acid；
(4) QDR nitrogen sparges：After pickling terminates, the polycrystalline bar in acid corrosion groove is taken out and is put into ultrasonic sink, this
Process needs to use nitrogen sparge to protect, and prevents polycrystalline bar surface oxidation；
(5) it is ultrasonic：By vibration of ultrasonic wave, the acid solution and impurity of polycrystalline billet surface are removed；
(6) dry：Hot-air seasoning polycrystalline bar；
(7) blanking：Polycrystalline bar is placed on blanking bench after wind drenches window.
7. a kind of large diameter zone melting according to claim 6 cleaning method of the cleaning device of polycrystalline bar, its feature
It is：The proportioning of the nitration mixture is that the volume ratio of nitric acid and hydrofluoric acid is 7.5：1.
8. a kind of large diameter zone melting according to claim 6 cleaning method of the cleaning device of polycrystalline bar, its feature
It is：A length of 3min during the nitrogen sparge.
9. a kind of large diameter zone melting according to claim 6 cleaning method of the cleaning device of polycrystalline bar, its feature
It is：A length of 15min when described ultrasonic.
10. a kind of large diameter zone melting according to claim 6 cleaning method of the cleaning device of polycrystalline bar, its feature
It is：The drying temperature is 60-90 DEG C, and drying time is 10-15min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410525225.9A CN104362114B (en) | 2014-09-30 | 2014-09-30 | A kind of large diameter zone melting cleaning device and its cleaning method of polycrystalline bar |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410525225.9A CN104362114B (en) | 2014-09-30 | 2014-09-30 | A kind of large diameter zone melting cleaning device and its cleaning method of polycrystalline bar |
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| CN104362114A CN104362114A (en) | 2015-02-18 |
| CN104362114B true CN104362114B (en) | 2017-07-18 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104624571B (en) * | 2015-03-04 | 2016-06-01 | 烽火通信科技股份有限公司 | The automatic tube cleaner of crystal reaction tube and automatically wash pipe method |
| CN109560006B (en) * | 2017-09-26 | 2023-10-20 | 天津环鑫科技发展有限公司 | Automatic source production line of scribbling of silicon chip |
| CN111151504A (en) * | 2020-01-19 | 2020-05-15 | 洛阳中硅高科技有限公司 | Polycrystalline silicon cleaning machine and method for cleaning polycrystalline silicon |
| CN111977988B (en) * | 2020-08-04 | 2021-06-08 | 湖南巨强再生资源科技发展有限公司 | Waste glass recycling production line based on horseshoe flame smelting furnace |
| CN112222097B (en) * | 2020-09-04 | 2022-03-08 | 山东国晶新材料有限公司 | Method for removing residues on surface of clamping rod |
| CN112959527B (en) * | 2021-02-05 | 2023-04-28 | 浙江快驴科技有限公司 | Battery intelligent management chip production and feeding device and use method |
| CN113319058A (en) * | 2021-06-16 | 2021-08-31 | 中国恩菲工程技术有限公司 | Polycrystalline silicon cleaning device |
| CN114226334A (en) * | 2021-12-29 | 2022-03-25 | 有研半导体硅材料股份公司 | Polycrystalline silicon rod cleaning device and method |
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| CN1395155A (en) * | 2001-07-05 | 2003-02-05 | 丽台科技股份有限公司 | Conversion device of DDR and QDR and adapter card, main board and internal memory module interface using it |
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