CN104630739A - Cleaning method of quartz tube in graphene growth furnace tube - Google Patents
Cleaning method of quartz tube in graphene growth furnace tube Download PDFInfo
- Publication number
- CN104630739A CN104630739A CN201510083034.6A CN201510083034A CN104630739A CN 104630739 A CN104630739 A CN 104630739A CN 201510083034 A CN201510083034 A CN 201510083034A CN 104630739 A CN104630739 A CN 104630739A
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- Prior art keywords
- silica tube
- graphene growth
- quartz tube
- tube
- kaolin
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4405—Cleaning of reactor or parts inside the reactor by using reactive gases
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4407—Cleaning of reactor or reactor parts by using wet or mechanical methods
Abstract
The invention relates to a cleaning method of a quartz tube in a graphene growth furnace tube. The method comprises the following steps: 1: heating a furnace body of a graphene growth furnace to 600-900 DEG C, keeping a constant temperature, simultaneously introducing oxygen into the quartz tube in the graphene growth furnace and lasting for 1-2 hours; 2 cooling the temperature in the graphene growth furnace to a room temperature, and wiping the inner wall of the quartz tube with kaolin containing ferric nitrate until attachment on the inner wall of the quartz tube disappears; 3 removing kaolin in the quartz tube, and wiping the overall cavity of the quartz tube with non-dust cloth for dipping alcohol; and 4 introducing nitrogen into the quartz tube for blowing after no residue exists in the quartz tube by virtue of visual inspection. According to the cleaning method, by virtue of an oxygen combustion method, a carbon material residue is removed; material residues on a growth substrate are removed by mechanical friction and a chemical reagent; a special cleaning machine does not need to be purchased; high equipment purchase expense is reduce; the quartz tube in the furnace body does not need to be dismantled; and the equipment maintenance time is shortened.
Description
Technical field
The present invention relates to Graphene Preparation equipment technical field, particularly relate to the purging method of the silica tube in a kind of graphene growth boiler tube.
Background technology
In graphene film industrialization, the chemical vapor deposition furnace tube device of graphene growth many employings semiconductor industry, for reaching industrialized level, the caliber of chemical vapor deposition device boiler tube is grown between 30cm to 45cm for graphene film, body of heater length is between 300cm to 400cm, after graphene growth furnace tube device uses some cycles, silica tube two-port wall remains with atrament, and purple material remains, atrament composition is carbon, and purple material is that the copper volatilized under high temperature is attached to silica tube inwall; A little atrament is had to remain in the middle of silica tube; Above-mentioned residue is too much, and can have a strong impact on graphene growth quality, therefore need regularly to go to clear up above-mentioned residue, according to semiconductor industry experience, cleaning dedicated quartz tube cleaning equipment, selects special chemical medicine company.Semiconductor industry adopts chemical vapor deposition boiler tube silica tube cleaning professional equipment price between 60 ten thousand to 90 ten thousand, and concerning the Graphene new industry primary stage, facility investment is very large; Bulky for graphene film growth chemical vapor deposition furnace tube device, the dismounting of cleaning silica tube is relative loaded down with trivial details with installation, length consuming time, easily occurs that silica tube is damaged in unloading process, and the damaged maintenance cost of silica tube is expensive; Cleaning boiler tube chemical liquids price, has corrosion risk to people; After having cleaned, chemical vapor deposition boiler tube time of answering a pager's call is long.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of simple efficient, method for cleaning silica tube in graphene growth boiler tube that cost is low.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: the purging method of the silica tube in a kind of graphene growth boiler tube, comprises the following steps:
Step one, is warming up to 600-900 DEG C by the body of heater of graphene growth stove and keeps constant temperature, passes into oxygen, time length 1-2 hour in the silica tube in graphene growth stove simultaneously;
Step 2, in the body of heater treating graphene growth stove, temperature is down to room temperature, uses the kaolin wiping silica tube inwall containing iron nitrate, until the dirt settling on silica tube inwall disappears;
Step 3, removes the kaolin in silica tube, uses the whole cavity of non-dust cloth wiping silica tube picking alcohol;
Step 4, after visual inspection noresidue in silica tube, passes into nitrogen purging in silica tube.
On the basis of technique scheme, the present invention can also do following improvement.
Further, the speed passing into oxygen in described step one is 1-4L/Min.
Further, be that kaolin to be put into mass concentration be that the iron nitrate solution of 20%-60% soaks after 20-40 minute and takes out containing the kleit preparation method of iron nitrate in described step 2.
Further, described kaolinic order number is 600 order-1200 orders.
Further, the time using the kaolin wiping silica tube inwall of iron nitrate in described step 2 is 10-20 minute.
Further, the speed passing into nitrogen in described step 4 is 1-4L/Min.
Further, the time passing into nitrogen in described step 4 is 10-30 minute.
The invention has the beneficial effects as follows: the present invention utilizes the characteristic of residue in silica tube after graphene growth, adopt the method for oxygen burnup, removing carbon species remains, utilize mechanical friction and chemical reagent to remove growth substrate material to remain, do not need buying Special cleaning board, save high equipment purchasing expense, do not need silica tube in dismounting body of heater, greatly save the maintenance of the equipment time, improve the output efficiency of equipment, use cheap chemical, save cost of equipment maintenance, be conducive to reducing products production cost, adopt human body without harm chemical treatments, avoid chemical to human injury's risk, board maintenance time can shorten greatly, indirect lifting board production efficiency.
Accompanying drawing explanation
Fig. 1 is schema of the present invention.
Embodiment
Be described principle of the present invention and feature below in conjunction with accompanying drawing, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment one
As shown in Figure 1, body of heater be warming up to 800 DEG C and keep constant temperature, the speed simultaneously with 2L/Min in silica tube passes into oxygen, 2 hours time length; Treat that in body of heater, temperature is down to room temperature, configuration quality concentration is the iron nitrate solution of 20%, 500 gram of 800 order kaolin is positioned in the iron nitrate solution prepared after soaking 30 minutes and takes out, use the kaolin wiping silica tube inwall containing iron nitrate, until the dirt settling on silica tube inwall disappears; Remove the kaolin in silica tube, use the whole cavity of non-dust cloth wiping silica tube picking alcohol; After visual inspection noresidue in silica tube, the speed with 2L/Min in silica tube passes into nitrogen purging, purges 15 minutes.
Embodiment two
As shown in Figure 1, body of heater be warming up to 600 DEG C and keep constant temperature, the speed simultaneously with 4L/Min in silica tube passes into oxygen, 1.5 hours time length; Treat that in body of heater, temperature is down to room temperature, configuration quality concentration is the iron nitrate solution of 60%, 800 gram of 600 order kaolin is positioned in the iron nitrate solution prepared after soaking 20 minutes and takes out, use the kaolin wiping silica tube inwall containing iron nitrate, until the dirt settling on silica tube inwall disappears; Remove the kaolin in silica tube, use the whole cavity of non-dust cloth wiping silica tube picking alcohol; After visual inspection noresidue in silica tube, the speed with 4L/Min in silica tube passes into nitrogen purging, purges 10 minutes.
Embodiment three
As shown in Figure 1, body of heater be warming up to 900 DEG C and keep constant temperature, the speed simultaneously with 1L/Min in silica tube passes into oxygen, 1 hour time length; Treat that in body of heater, temperature is down to room temperature, configuration quality concentration is the iron nitrate solution of 40%, 300 gram of 1200 order kaolin is positioned in the iron nitrate solution prepared after soaking 40 minutes and takes out, use the kaolin wiping silica tube inwall containing iron nitrate, until the dirt settling on silica tube inwall disappears; Remove the kaolin in silica tube, use the whole cavity of non-dust cloth wiping silica tube picking alcohol; After visual inspection noresidue in silica tube, the speed with 1L/Min in silica tube passes into nitrogen purging, purges 30 minutes.
The present invention utilizes the characteristic of residue in silica tube after graphene growth, adopt the method for oxygen burnup, removing carbon species remains, carbon species under the condition of high temperature with the oxygen reaction passed into, generate carbon monoxide and carbon dioxide, under the drive along with the oxysome passed into, discharge silica tube; Utilize mechanical friction and chemical reagent to remove growth substrate material to remain, adhere to iron nitrate on the kaolin to react with residual growth substrate in the process of friction, remove residue, the kaolinic Certain residues removed and stick on silica tube tube wall that can rub on the one hand that rubs, another side can accelerate the speed of reaction of iron nitrate and residue.The present invention does not need buying Special cleaning board, save high equipment purchasing expense, do not need silica tube in dismounting body of heater, greatly save the maintenance of the equipment time, improve the output efficiency of equipment, use cheap chemical, saved cost of equipment maintenance, be conducive to reducing products production cost, adopt human body without harm chemical treatments, avoid chemical to human injury's risk, board maintenance time can shorten greatly, indirectly promotes board production efficiency.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. a purging method for the silica tube in graphene growth stove, is characterized in that, comprise the following steps:
Step one, is warming up to 600-900 DEG C by the body of heater of graphene growth stove and keeps constant temperature, passes into oxygen, time length 1-2 hour in the silica tube in graphene growth stove simultaneously;
Step 2, in the body of heater treating graphene growth stove, temperature is down to room temperature, uses the kaolin wiping silica tube inwall containing iron nitrate, until the dirt settling on silica tube inwall disappears;
Step 3, removes the kaolin in silica tube, uses the whole cavity of non-dust cloth wiping silica tube picking alcohol;
Step 4, after visual inspection noresidue in silica tube, passes into nitrogen purging in silica tube.
2. the purging method of the silica tube in a kind of graphene growth boiler tube according to claim 1, is characterized in that, the speed passing into oxygen in described step one is 1-4L/Min.
3. the purging method of the silica tube in a kind of graphene growth boiler tube according to claim 1, it is characterized in that, be that kaolin to be put into mass concentration be that the iron nitrate solution of 20%-60% soaks after 20-40 minute and takes out containing the kleit preparation method of iron nitrate in described step 2.
4. the purging method of the silica tube in a kind of graphene growth boiler tube according to claim 1, is characterized in that, described kaolinic order number is 600 order-1200 orders.
5. the purging method of the silica tube in a kind of graphene growth boiler tube according to claim 1, is characterized in that, the time using the kaolin wiping silica tube inwall of iron nitrate in described step 2 is 10-20 minute.
6. the purging method of the silica tube in a kind of graphene growth boiler tube according to claim 1, is characterized in that, the speed passing into nitrogen in described step 4 is 1-4L/Min.
7. the purging method of the silica tube in a kind of graphene growth boiler tube according to claim 1, is characterized in that, the time passing into nitrogen in described step 4 is 10-30 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510083034.6A CN104630739B (en) | 2015-02-15 | 2015-02-15 | A kind of cleaning method of quartz ampoule in graphene growth boiler tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510083034.6A CN104630739B (en) | 2015-02-15 | 2015-02-15 | A kind of cleaning method of quartz ampoule in graphene growth boiler tube |
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| CN104630739A true CN104630739A (en) | 2015-05-20 |
| CN104630739B CN104630739B (en) | 2017-08-18 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106929824A (en) * | 2015-12-29 | 2017-07-07 | 中国建材国际工程集团有限公司 | The method and apparatus and coating facility of substrate transport establishment in cleaning coating facility |
| CN111348936A (en) * | 2018-12-21 | 2020-06-30 | 汉能新材料科技有限公司 | Crucible oxidation device and oxidation method |
| CN113020133A (en) * | 2021-04-27 | 2021-06-25 | 山西钢科碳材料有限公司 | Cleaning method of polyacrylonitrile carbon fiber precursor drying densification equipment |
| CN114289420A (en) * | 2022-02-21 | 2022-04-08 | 常州二维碳素科技股份有限公司 | Method for removing carbon deposit on inner wall of air inlet pipe in CVD (chemical vapor deposition) grown graphene powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06145990A (en) * | 1992-11-10 | 1994-05-27 | Hitachi Electron Eng Co Ltd | Cleaning method for cvd apparatus |
| CN1388229A (en) * | 2002-06-13 | 2003-01-01 | 山东中纳新能源科技有限公司 | Efficient nano fuel coal reinforcer and its prepn |
| CN101301611A (en) * | 2008-07-07 | 2008-11-12 | 西南化工研究设计院 | Sulfur-tolerance deoxidation catalyst and preparation and use thereof |
| CN103599746A (en) * | 2013-11-04 | 2014-02-26 | 中国科学院合肥物质科学研究院 | Method for preparing natural ore soil loaded nanometer arsenic removal agent |
-
2015
- 2015-02-15 CN CN201510083034.6A patent/CN104630739B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06145990A (en) * | 1992-11-10 | 1994-05-27 | Hitachi Electron Eng Co Ltd | Cleaning method for cvd apparatus |
| CN1388229A (en) * | 2002-06-13 | 2003-01-01 | 山东中纳新能源科技有限公司 | Efficient nano fuel coal reinforcer and its prepn |
| CN101301611A (en) * | 2008-07-07 | 2008-11-12 | 西南化工研究设计院 | Sulfur-tolerance deoxidation catalyst and preparation and use thereof |
| CN103599746A (en) * | 2013-11-04 | 2014-02-26 | 中国科学院合肥物质科学研究院 | Method for preparing natural ore soil loaded nanometer arsenic removal agent |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106929824A (en) * | 2015-12-29 | 2017-07-07 | 中国建材国际工程集团有限公司 | The method and apparatus and coating facility of substrate transport establishment in cleaning coating facility |
| CN111348936A (en) * | 2018-12-21 | 2020-06-30 | 汉能新材料科技有限公司 | Crucible oxidation device and oxidation method |
| CN113020133A (en) * | 2021-04-27 | 2021-06-25 | 山西钢科碳材料有限公司 | Cleaning method of polyacrylonitrile carbon fiber precursor drying densification equipment |
| CN114289420A (en) * | 2022-02-21 | 2022-04-08 | 常州二维碳素科技股份有限公司 | Method for removing carbon deposit on inner wall of air inlet pipe in CVD (chemical vapor deposition) grown graphene powder |
| CN114289420B (en) * | 2022-02-21 | 2023-09-01 | 常州二维碳素科技股份有限公司 | Method for removing carbon deposition on inner wall of air inlet pipe in CVD (chemical vapor deposition) grown graphene powder |
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| CN104630739B (en) | 2017-08-18 |
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