CN103894381A - Furnace pipe cleaning method - Google Patents

Furnace pipe cleaning method Download PDF

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Publication number
CN103894381A
CN103894381A CN201410106604.4A CN201410106604A CN103894381A CN 103894381 A CN103894381 A CN 103894381A CN 201410106604 A CN201410106604 A CN 201410106604A CN 103894381 A CN103894381 A CN 103894381A
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China
Prior art keywords
boiler tube
oxygen
cleaning method
furnace pipe
dichloroethylene
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CN201410106604.4A
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Chinese (zh)
Inventor
江润峰
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Shanghai Huali Microelectronics Corp
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Shanghai Huali Microelectronics Corp
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Priority to CN201410106604.4A priority Critical patent/CN103894381A/en
Publication of CN103894381A publication Critical patent/CN103894381A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto 
    • B08B9/02—Cleaning pipes or tubes or systems of pipes or tubes
    • B08B9/027—Cleaning the internal surfaces; Removal of blockages

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Cleaning Or Drying Semiconductors (AREA)

Abstract

The invention discloses a furnace pipe cleaning method and relates to the microelectronic field. The method includes the steps that oxygen is introduced into the furnace pipe; nitrogen carrying dichloroethylene is injected into the furnace pipe for 55 minutes to 65 minutes; nitrogen injection is stopped; water steam is introduced into the furnace pipe; introducing of water steam is stopped. According to the method, alkali metal ions and remaining organic matter in the furnace pipe can be removed through the dichloroethylene and the oxygen at high temperature; due to the fact that the oxygen is introduced into the furnace pipe for a long time, and remaining dichloroethylene in the furnace pipe is removed; heavy metal ions in the furnace pipe are removed through the water steam. Heavy metal accumulated in the furnace pipe is removed with the method, the remaining dichloroethylene in the furnace pipe is removed, and the stability of subsequent processes is improved.

Description

A kind of boiler tube cleaning method
Technical field
The present invention relates to microelectronic, relate in particular to a kind of boiler tube cleaning method.
Background technology
Along with chip fabrication techniques development, semiconductor silicon chip size is increasing, technology requirement is more and more stricter, and the effect of boiler tube periodic cleaning is had higher requirement.Simple boiler tube cleans and can not meet actual production application, particularly metallic pollution is had the device products of requirements at the higher level.Conventionally chip manufacturing will be passed through the process repeatedly such as cleaning, diffusion technique, injection technology, photoetching process, etching technics, carrying out repeatedly after film forming, residue metal ion and high molecular polymer remnants in boiler tube are cumulative, if irregularly removed, metallic pollution and particle source be may form, thereby technique yield and product stability affected.
In boiler tube, requisite parts have quartz ampoule (quarz tube) and brilliant boat (boat).Conventionally the material of quartz ampoule is quartz, and brilliant boat material has two kinds of quartz or SiC.Table 1 is the tenor of the brilliant boat of parts SiC and quartz ampoule in boiler tube.
Table 1
? Na K AL Fe Cu Mg Ca
The brilliant boat of SiC (ppm) 1.0 1.0 15.0 10.0 1.0 1.0 2.0
Quartz ampoule (ppm) 0.5 1.0 25.0 1.0 0.5 1.0 2.0
Wherein, ppm represents solution concentration.
Metallic pollution has the impact of semiconductor devices: metal impurities are easily at Si-SiO 2interface formation is built up, and affects gate oxide integrity (Gate Oxide Integrity is called for short GOI), reduces oxide breakdown voltage (Oxide breakdown voltage is called for short BV-OX), device is formed and leak (Leakage).Particularly beavy metal impurity is particularly responsive to metal impurities for CMOS analog sensor (CMOS Imagine Sensor is called for short CIS) product, easily produces dark current (Dark current is called for short DC), causes white-spot defects (White Spot Defect).
Metal ion under hot conditions has higher diffusion coefficient in silicon and silica, so after the long-time high-temperature operation of boiler tube, current technique causes that the metallic pollution that (parts of quartz or carborundum) metallic pollution or previous process are brought into is easily diffused into silicon chip inside, be difficult to remove by cleaning, thereby form permanent defect.So boiler tube board must carry out regular cleaning.
Traditional boiler tube ablution has:
N2 cleans, and under high temperature, N2 can remove granule and the organic matter remnants in boiler tube, but can not remove metal ion;
Chlorion cleans, and usually adopt the Cl in dichloroethylene (Trans-LC, TCA) or HCl to remove residual metal ion, but due to environmental protection and security consideration, TCA and HCl is slowly eliminated;
At present the most frequently used is that dichloroethylene (Trans-LC) cleans, and Trans-LC is a kind of liquid, and Trans-LC is carried and enters boiler tube by nitrogen, under high temperature, generates HCl with oxygen reaction, and HCl plays the effect that purifies boiler tube.Chemical reaction equation is:
C2H2Cl2+O2→2HCl+2CO2
At 800～1100 degree, boiler tube is carried out to Trans-LC about 1 hour and clean, can effectively get rid of the alkali metal ions such as Na/K and organic matter.But at high temperature HCl easily takes the trace of Al/Fe/Cu/Ca in boiler tube parts out of simultaneously, and HCl can not remove heavy metals such as Al/Fe/Cu/Ca, easily forms Heavy Metal Accumulation.Cleaning itself easily has the remnants of Trans-LC or HCl, and these remnants cause bad impact to follow-up technique, such as HCL remnants make oxidated layer thickness thickening, causes technique shakiness.
Chinese patent (CN103372559A) discloses a kind of boiler tube cleaning method, comprises the steps: boiler tube to heat up; In boiler tube, pass into dichloroethylene to remove movable metal ion; In boiler tube, pass into oxygen to remove residual dichloroethylene.
This patent is removed the residual of dichloroethylene by pass into oxygen after dichloroethylene purges, and makes boiler tube can carry out immediately next step production after quality control, does not worry the residual problem of bringing of dichloroethylene.But do not solve Heavy Metal Accumulation, and because producing the remaining problem that affects subsequent technique shakiness of Trans-LC or HCl.
Chinese patent (CN101327487B) discloses a kind of cleaning method and system of boiler tube, and nitrogen is passed into cleaning agent groove, utilizes nitrogen to carry described cleaning agent and passes into described boiler tube through a pipeline, and described boiler tube is cleaned; To after hydrogen and oxygen mix generation water vapour, by boiler tube, described boiler tube be cleaned.
The boiler tube cleaning method of this patent can be removed metal and the nonmetallic inclusion deposit of boiler tube inside in semiconductor oxide boiler tube equipment effectively.But do not solve Heavy Metal Accumulation, and because producing the remaining problem that affects subsequent technique shakiness of Trans-LC or HCl.
Summary of the invention
There is easily formation Heavy Metal Accumulation for solving prior art in the present invention, and produces Trans-LC or HCl remnants, thereby affect the problem of subsequent technique shakiness, thereby a kind of technical scheme of boiler tube cleaning method is provided.
A kind of boiler tube cleaning method of the present invention, comprises the steps:
Step 1. passes into oxygen to boiler tube;
Step 2. is injected the nitrogen that carries dichloroethylene of 55～65 minutes to described boiler tube;
Step 3. stops injecting described nitrogen;
Step 4. passes into aqueous vapor to described boiler tube;
Step 5. stops passing into described aqueous vapor.
Preferably, the temperature of described boiler tube is 900 ℃～1000 ℃.
Preferably, the described oxygen time passing into described boiler tube in step 1 is 5～10 minutes.
Preferably, aqueous vapor described in step 4 is that volume ratio is that the hydrogen of 1:1 and described oxygen pass into the described aqueous vapor generating to combustion chamber.
Preferably, the time that passes into described aqueous vapor to described boiler tube in step 4 is 55～65 minutes.
Preferably, the process that stops passing into described aqueous vapor in step 5 is: first stop passing into of described hydrogen, then stop passing into of described oxygen.
Preferably, stop described hydrogen pass into 5 minutes after stop passing into of oxygen.
Preferably, the step that passes into described oxygen, described hydrogen and described nitrogen is carried out by the menu control of the mass flow controller of board.
Beneficial effect of the present invention:
This method at high temperature can be removed alkali metal ion and organic matter remnants in boiler tube by dichloroethylene and oxygen; The remnants of dichloroethylene in boiler tube are removed by passing into for a long time oxygen; Remove the heavy metal ion in boiler tube by aqueous vapor.The present invention has eliminated the heavy metal of accumulating in boiler tube, and has removed the remnants of dichloroethylene in boiler tube, has reached the object of the stability that has improved subsequent technique.
Accompanying drawing explanation
Fig. 1 is the method flow diagram that boiler tube of the present invention cleans;
Fig. 2 is the apparatus structure schematic diagram that boiler tube cleans.
In accompanying drawing: 1. the first valve; 2. the second valve; 3. the 3rd valve; 4. the 4th valve; A. oxygen; B. hydrogen; C. nitrogen; D. dichloroethylene solution; E. combustion chamber; F. air inlet; G. boiler tube; H. exhaust outlet.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described, but not as limiting to the invention.
The invention provides a kind of boiler tube cleaning method, a kind of embodiment is: brilliant boat is risen up in quartz reaction cavity, comprise the steps: as depicted in figs. 1 and 2,
Step 1. is the boiler tube G of 900 ℃～1000 ℃ to temperature, open the first valve 1, by air inlet F, oxygen A is delivered to boiler tube G, the oxygen A time passing into is 5～10 minutes, make boiler tube G in the state of oxidation, prevent at high temperature carbonization of dichloroethylene (Trans-LC), produce particle contamination, waste gas is discharged by exhaust outlet H;
Step 2. continues to keep oxygen A to pass into, open the 4th valve 4 and the 3rd valve 3 simultaneously, air admission hole is injected into nitrogen C in dichloroethylene solution D, by venthole, the nitrogen C that carries dichloroethylene is passed into boiler tube G, the time of passing into is 55～65 minutes, and dichloroethylene and oxygen A at high temperature can remove alkali metal ion and organic matter remnants in boiler tube G;
Step 3. stops nitrogen injection C, closes the 4th valve 4 and the 3rd valve 3, continues to keep oxygen A to pass into, and continues to keep oxygen A to pass into the remnants that can remove dichloroethylene, prevents again the follow-up excessive problem of hydrogen B;
Step 4. passes into aqueous vapor to boiler tube G, opens the second valve 2, and the hydrogen B that is 1:1 by volume ratio and oxygen A pass into combustion chamber E, high-purity aqueous vapor that igniting generates, the time that passes into aqueous vapor to boiler tube G is 55～65 minutes, and aqueous vapor can heavy-metal ion removal, further removes dichloroethylene remnants;
Hydrogen B and the chemical equation of oxygen A in the E of combustion chamber are:
2H 2+O 2→2H 2O；
Step 5. stops passing into aqueous vapor, and detailed process is: first close the second valve 2, stop passing into of hydrogen B, close the first valve 1 again and stop passing into of oxygen A after 5 minutes, prevent that hydrogen is excessive.
The above-mentioned step of oxygen, hydrogen and nitrogen that passes into is carried out or is controlled by valve (valve) by the menu control of the mass flow controller of board (MFC).
Can realize by control wafer being positioned over to the mode of San Ge position, upper, middle and lower of boiler tube the monitoring that boiler tube is cleaned.According to the icp ms of control wafer (ICPMS) testing result, metallic pollution is carried out to off-line (offline) assessment.Result shows that boiler tube cleaning method of the present invention has the improvement of an order of magnitude to metallic pollution.
As shown in table 2, carry out (Inline) assessment online according to concentration of metal ions and carrier diffusion length result.Control wafer is used after new technology, and the concentration of metal ions of control wafer reduces, carrier diffusion length is elongated, all shows that this boiler tube cleaning method has greatly improved to removing metallic pollution and organic remnants, has reduced metallic pollution.
Table 2
Figure BDA0000479926370000071
The foregoing is only preferred embodiment of the present invention; not thereby limit embodiments of the present invention and protection domain; to those skilled in the art; the scheme that being equal to of should recognizing that all utilizations description of the present invention and diagramatic content done replaces and apparent variation obtains, all should be included in protection scope of the present invention.

Claims (8)

1. a boiler tube cleaning method, is characterized in that, comprises the steps:
Step 1. passes into oxygen to boiler tube;
Step 2. is injected the nitrogen that carries dichloroethylene of 55～65 minutes to described boiler tube;
Step 3. stops injecting described nitrogen;
Step 4. passes into aqueous vapor to described boiler tube;
Step 5. stops passing into described aqueous vapor.
2. boiler tube cleaning method as claimed in claim 1, is characterized in that, the temperature of described boiler tube is 900 ℃～1000 ℃.
3. boiler tube cleaning method as claimed in claim 1, is characterized in that, the described oxygen time passing into described boiler tube in step 1 is 5～10 minutes.
4. boiler tube cleaning method as claimed in claim 1, is characterized in that, aqueous vapor described in step 4 is that volume ratio is that hydrogen and the described oxygen of 1:1 passes into the described aqueous vapor generating to combustion chamber.
5. boiler tube cleaning method as claimed in claim 1, is characterized in that, the time that passes into described aqueous vapor to described boiler tube in step 4 is 55～65 minutes.
6. boiler tube cleaning method as claimed in claim 1, is characterized in that, the process that stops passing into described aqueous vapor in step 5 is: first stop passing into of described hydrogen, then stop passing into of described oxygen.
7. boiler tube cleaning method as claimed in claim 6, is characterized in that, stop described hydrogen pass into 5 minutes after stop passing into of oxygen.
8. boiler tube cleaning method as described in any one in claim 1 to 7, is characterized in that, the step that passes into described oxygen, described hydrogen and described nitrogen is carried out by the menu control of the mass flow controller of board.
CN201410106604.4A 2014-03-20 2014-03-20 Furnace pipe cleaning method Pending CN103894381A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104259153A (en) * 2014-07-24 2015-01-07 上海华力微电子有限公司 Furnace tube cleaning process
CN105225936A (en) * 2015-10-14 2016-01-06 上海华力微电子有限公司 A kind of method of thickness of grid oxide layer of eliminating the effects of the act and device
CN106298616A (en) * 2015-06-04 2017-01-04 有研半导体材料有限公司 A kind of silicon chip load bearing component and the method reducing high annealing sheet metal content
CN107331728A (en) * 2017-06-20 2017-11-07 常州亿晶光电科技有限公司 The technique for improving PERC high-efficiency battery EL yields
CN108198909A (en) * 2018-01-15 2018-06-22 浙江晶科能源有限公司 A kind of silicon slice processing method and solar cell production method
CN111089493A (en) * 2019-12-24 2020-05-01 通威太阳能（安徽）有限公司 Cleaning method for solar cell annealing furnace pipe
CN111974773A (en) * 2019-05-23 2020-11-24 中国科学院大连化学物理研究所 Method for cleaning air bag for collecting exhaled air
CN112570393A (en) * 2019-09-27 2021-03-30 长鑫存储技术有限公司 Furnace tube cleaning method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1285954A (en) * 1998-01-07 2001-02-28 Memc电子材料有限公司 In situ wafer cleaning process
US7172657B2 (en) * 2000-03-10 2007-02-06 Tokyo Electron Limited Cleaning method of treatment equipment and treatment equipment
JP2009231332A (en) * 2008-03-19 2009-10-08 Toyoko Kagaku Co Ltd Cleaning gas supply device and semiconductor processing apparatus
CN101327487B (en) * 2007-06-21 2010-12-22 中芯国际集成电路制造(上海)有限公司 Method and system for cleaning boiler tube
CN102825036A (en) * 2012-08-23 2012-12-19 英利能源（中国）有限公司 Cleaning method for furnace tube for diffusion
CN103372559A (en) * 2012-04-24 2013-10-30 无锡华润上华科技有限公司 Cleaning method for furnace tube

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1285954A (en) * 1998-01-07 2001-02-28 Memc电子材料有限公司 In situ wafer cleaning process
US7172657B2 (en) * 2000-03-10 2007-02-06 Tokyo Electron Limited Cleaning method of treatment equipment and treatment equipment
CN101327487B (en) * 2007-06-21 2010-12-22 中芯国际集成电路制造(上海)有限公司 Method and system for cleaning boiler tube
JP2009231332A (en) * 2008-03-19 2009-10-08 Toyoko Kagaku Co Ltd Cleaning gas supply device and semiconductor processing apparatus
CN103372559A (en) * 2012-04-24 2013-10-30 无锡华润上华科技有限公司 Cleaning method for furnace tube
CN102825036A (en) * 2012-08-23 2012-12-19 英利能源（中国）有限公司 Cleaning method for furnace tube for diffusion

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104259153A (en) * 2014-07-24 2015-01-07 上海华力微电子有限公司 Furnace tube cleaning process
CN106298616A (en) * 2015-06-04 2017-01-04 有研半导体材料有限公司 A kind of silicon chip load bearing component and the method reducing high annealing sheet metal content
CN106298616B (en) * 2015-06-04 2019-12-13 有研半导体材料有限公司 Silicon wafer bearing part and method for reducing metal content of high-temperature annealing sheet
CN105225936A (en) * 2015-10-14 2016-01-06 上海华力微电子有限公司 A kind of method of thickness of grid oxide layer of eliminating the effects of the act and device
CN107331728A (en) * 2017-06-20 2017-11-07 常州亿晶光电科技有限公司 The technique for improving PERC high-efficiency battery EL yields
CN107331728B (en) * 2017-06-20 2019-09-03 常州亿晶光电科技有限公司 The technique for improving PERC high-efficiency battery EL yield
CN108198909A (en) * 2018-01-15 2018-06-22 浙江晶科能源有限公司 A kind of silicon slice processing method and solar cell production method
CN108198909B (en) * 2018-01-15 2020-04-14 浙江晶科能源有限公司 Silicon wafer processing method and solar cell manufacturing method
CN111974773A (en) * 2019-05-23 2020-11-24 中国科学院大连化学物理研究所 Method for cleaning air bag for collecting exhaled air
CN111974773B (en) * 2019-05-23 2022-04-12 中国科学院大连化学物理研究所 Method for cleaning air bag for collecting exhaled air
CN112570393A (en) * 2019-09-27 2021-03-30 长鑫存储技术有限公司 Furnace tube cleaning method
CN111089493A (en) * 2019-12-24 2020-05-01 通威太阳能（安徽）有限公司 Cleaning method for solar cell annealing furnace pipe

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Application publication date: 20140702