CN101502835A - Method for cleaning graphite base in MOCVD equipment - Google Patents
Method for cleaning graphite base in MOCVD equipment Download PDFInfo
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- CN101502835A CN101502835A CNA2009101149154A CN200910114915A CN101502835A CN 101502835 A CN101502835 A CN 101502835A CN A2009101149154 A CNA2009101149154 A CN A2009101149154A CN 200910114915 A CN200910114915 A CN 200910114915A CN 101502835 A CN101502835 A CN 101502835A
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Abstract
The invention discloses a cleaning method of graphite base in MOCVD apparatus. The method is used for cleaning the graphite base in the MOCVD apparatus and can completely clean the graphite base cleanly, in particular the attachments in small pits on the surface of the graphite base without damaging the structure of the graphite base, so as to prolong the service life of the graphite base and improve the productivity of the MOCVD apparatus. The method comprises the steps of boiling in acid, specifically, putting the graphite base in phosphoric acid for boiling until the attachments on the surface of the graphite base are removed completely, then taking out the graphite base, and the step of boiling in acid further comprises the process of brushing off the attachments on the surface of the graphite base; water-flushing, specifically, flushing the well boiled graphite base by hot de-ionized water to remove acidic substances on the graphite base; and drying, specifically, drying the graphite base until the graphite base thereon has no moisture. The drying step comprises the process of drying the graphite base in a roasting manner. The invention uses the way of wet treatment.
Description
Technical field
The present invention relates to the graphite base in a kind of MOCVD equipment, particularly relate to the cleaning method of graphite base.
Background technology
MOCVD (metal organic-matter chemical gaseous phase deposition) equipment is as the means of compound semiconductor materials research and production, and particularly as the equipment of suitability for industrialized production, it is that other semiconductor equipment is irreplaceable.Its high-quality, stability, repeatability and multifunctionality are more and more paid attention to by people.It is the main means of producing semiconductor photoelectric device and microwave device material in the world today, as laser instrument, light emitting diode, high performance solar batteries, photocathode etc., is the indispensable equipment of industry such as photoelectron.
After MOCVD equipment comprises that the graphite base that is used to settle with heated substrate is using certain number of times, can on graphite base, form sediment, sediment is wrapped in the heat conduction that influences graphite on the graphite base, simultaneously attached to the sediment on the graphite base in follow-up heated products manufacture process, product is formed pollution, influence product quality.
Be to strike off top attachment to the method for cleaning commonly used of the graphite substrate in the MOCVD equipment at present.Graphite base is made up of the graphite of inside and the SiC on top layer, because the manufacture craft of graphite base causes the pitting that a lot of depressions are arranged on the SiC layer, by the method for striking off, can not wipe the attachment in the pit off, destroy the SiC layer again easily if excessively strike off attachment, influence the service life of graphite base.
Summary of the invention
Technical problem to be solved by this invention provides the cleaning method of graphite base in a kind of MOCVD equipment, this method is used for cleaning the graphite base of MOCVD equipment, can completely graphite base be cleaned up by this method, the attachment in the pitting on graphite base surface particularly, and do not destroy the structure of graphite base, thereby play service life that prolongs graphite base and the effect that improves the MOCVD equipment capacity.
In order to solve technical problem of the present invention, the present invention proposes the cleaning method of graphite base in a kind of MOCVD equipment, and this method may further comprise the steps:
Boil acid: graphite base is put into phosphoric acid boil, be removed clean the back to the lip-deep attachment of graphite base and take out, wherein, describedly boil sour step and also comprise the attachment that brushes away the graphite base surface;
Bath: clean well-done graphite base with hot deionized water, remove the acidic materials on the graphite base;
Dry: dry graphite base, exclusion to the graphite base, wherein, described drying steps comprises with the dry graphite base of roasting mode.
Preferably: carry out described boil sour step after, inhale and go acid solution on the graphite base with inhaling article that acid wipes acid, carry out described bath step again.Inhale and go that acid solution can reduce bath number of times and water consumption on the graphite base with inhaling article that acid wipes acid such as absorbent cotton, optimized whole flow process.
Preferably, describedly boil sour step and comprise: graphite base is put into phosphoric acid boil a period of time, take out the brush graphite base then, the part attachment on the graphite base is removed, put into phosphoric acid again and continue to boil.Boil in the sour process, graphite base is carried out above-mentioned processing, can not touch under the situation of the pitting on the SiC layer, plastic soft brush of graphite base top layer attachment with acid-proof brushed away.This step of attachment that brushes away the graphite base surface can be placed on above-mentioned boiling in the sour process carries out, and also can be placed on and boil carrying out at last of sour process.
Preferably, described bath step comprises swinging and washes and rinsing step; Wherein swing and wash step and comprise: the obverse and reverse of graphite base is swung wash, with inhaling the article that acid wipes acid graphite base is wiped then, continue again to swing and wash.Can make the acid-treated attachment of process in the pitting on the stone SiC layer become looser by swinging the mode of washing shake, and the acid substance that adheres in the pitting on the dilute Si C layer, to reduce the water consumption of follow-up rinsing step, and reach the effect of removing attachment preferably, to wiping of graphite base remaining acid substance and attachment in the SiC layer pitting are farthest reduced with the article of inhaling acid wiping acid, easier being removed in the process of washing of swinging in the back.Optimal way wherein is: described swinging washes that step comprises earlier successively front, the back of graphite base, the front is swung and washed one time again, repeats said process 5 times; With the article of inhaling acid wiping acid graphite base is wiped then; Swing again and wash one time.
Preferably, described rinsing step comprises: will swing washed graphite base and put into the bath groove, and with the hot deionized water flushing, and need taking-up to swing the shampooing suction in the flushing process.In process, swing and wash graphite base,, make the attachment in the pitting on the SiC layer break away from the surface of graphite base greatly, can reduce the time and the water consumption of bath, optimized developing technique by the vibration graphite base with the hot deionized water flushing.
Preferably: describedly inhale that article that acid wipes acid can be that degreasing cotton, chemicals absorption are cotton, in the dust-free paper any.
Preferably: described drying steps comprises that elder generation dries up graphite base, toasts again.Can use nitrogen gun blown graphite pedestal earlier, blow away the bulky grain globule of graphite base surface attachment, these removed bulky grain globules can be taken away the acid substance that is dissolved in the globule simultaneously, and in subsequent step, passing through can residual acid substance still less on the graphite base of drying like this.Acid substance remains in the pitting of SiC layer, in the process of baking, can corrode the SiC layer, and serious meeting causes the perforation of SiC layer, and graphite is come out, and the graphite of exposure can participate in reaction in the gaseous phase deposition process, thus rotten scrapping.
Preferably: the described water temperature of washing of swinging is 55 degrees centigrade～65 degrees centigrade, and the water temperature of described flushing is 70 degrees centigrade～100 degrees centigrade.Swinging the temperature of washing should not be too high, swings the purpose of washing and be the mode by vibration, is that water with the graphite base surface relative gentle friction takes place, thereby makes the interior acid attachment of pitting on the SiC layer become loose, and too high water temperature wastes energy.It is higher that the water temperature of flushing is swung the temperature of washing, and the acidic materials that help the graphite base surface are diffused in the water.
Preferably: the described temperature of acid of boiling is at 80 degrees centigrade～150 degrees centigrade; The temperature of described baking is at 60 degrees centigrade～180 degrees centigrade.
Beneficial effect of the present invention is as follows:
The mode that the graphite base surface attachments is struck off compared to existing technology, what the present invention adopted is a kind of mode of wet-treating.This method can effectively be removed the attachment on graphite base surface, and is particularly very good to the removal effect of attachment in the SiC layer pitting of graphite surface.This method can be when removing the graphite base surface attachments, and the SiC layer on protection graphite base top layer is not destroyed, and then has protected the graphite of internal layer, and it can prolong the service life of graphite base and the effect that improves the MOCVD equipment capacity.
The specific embodiment
The invention provides the cleaning method of graphite base in a kind of MOCVD equipment.
Embodiment one:
Earlier graphite base is inserted in 70 degrees centigrade～93 degrees centigrade the phosphoric acid and boil, take out then, with the surface of the plastic soft brush brush graphite base of acid-proof, remove the attachment on graphite base surface, put into phosphoric acid again and continue to boil, take out again, clean down with the attachment of brush with the graphite base surface.If the graphite base surface is still unclean, just repeat the above-mentioned step of boiling and brushing.Graphite base boils after acid finishes, and wipes graphite base with degreasing cotton, wipes the acid solution on graphite base surface.
Put into 70 degrees centigrade hot deionized water flushing 10 times with boiling graphite base after the acid; Steep then in 70 degrees centigrade hot deionized water, changed water once in per 1 hour, change water altogether 18 times; Steep a night then.
Took out graphite base, and graphite base was dried up in second day with nitrogen gun; Put into baking oven then, dry by the fire half an hour under 90 degrees centigrade environment, dry by the fire half an hour in 120 degrees centigrade environment, baking is 15 hours in 180 degrees centigrade environment.
Embodiment two:
Earlier graphite base is inserted in 125 degrees centigrade of phosphoric acid and boil, boil 21 minutes (according to the attachment situation of graphite base) back and take out, brush away the attachment on graphite base surface.
Graphite base is put into the bath groove, use 70 degrees centigrade hot deionized water flushing to take out after 32 hours.
Then graphite base is inserted in the baking oven and toasted 0.5 hour under 90 degrees centigrade of situations, baking is 1 hour under 110 degrees centigrade of situations, and baking is 15 hours under 180 degrees centigrade of situations.
Embodiment three:
Earlier graphite base is inserted and boiled in 80 degrees centigrade of phosphoric acid 2 hours 50 minutes, brush away the attachment on graphite base surface after the taking-up.Inhale immediately with degreasing cotton again and wipe one time.
Dash 5 times 60 degrees centigrade of water temperatures then with hot deionized water; Be immersed in the water again, changed water one time in per 1 hour, change water 26 times, water temperature is controlled at 90 degrees centigrade.
Baking is dry then.Baking temperature is slowly adjusted to 180 degrees centigrade by 60 degrees centigrade, and front and back continue 4 hours.
Embodiment four:
The phosphoric acid of earlier graphite base being put into 140 degrees centigrade～150 degrees centigrade boiled 70 minutes more, brush away the attachment on graphite base surface then with brush, if still have attachment, just continue that graphite base is put into phosphoric acid and boil, up to brush with the graphite base surface brush clean till.
Take out graphite base then, wipe the acid solution of graphite surface.
Again graphite base is washed by water.Water is 60 degrees centigrade hot deionized water, and the bath step is specially:
1, earlier the front of graphite base is swung wash one time, then the back of graphite base is swung wash one time, the front of graphite base swung again wash one time again, repeat said process 5 times; Wipe the surface of graphite base then with degreasing cotton, swing and wash the back and take out putting into hot deionized water then.
2, wash graphite base being put into the bath groove then, uses 99 degrees centigrade hot deionization flushing 20 hours, wherein, swing to wash every 1 hour taking-up graphite base and wipe once.
After finishing the bath step, with nitrogen gun the water on the graphite base is dried up earlier, again graphite base is put into baking oven, baking temperature is adjusted to 180 degrees centigrade by 90 degrees centigrade of 90 degrees centigrade of branches, 110 degrees centigrade and 180 degrees centigrade of three phases, and front and back continue 2 hours.
Through the graphite base of above-mentioned processing, the pitting on its SiC layer is cleaned very totally.
Claims (10)
1, the cleaning method of graphite base in a kind of MOCVD equipment is characterized in that may further comprise the steps:
Boil acid: graphite base is put into phosphoric acid boil, be removed clean the back to the lip-deep attachment of graphite base and take out, wherein, describedly boil sour step and also comprise the attachment that brushes away the graphite base surface;
Bath: clean well-done graphite base with hot deionized water, remove the acidic materials on the graphite base;
Dry: dry graphite base, exclusion to the graphite base, wherein, described drying steps comprises with the dry graphite base of roasting mode.
2, the cleaning method of graphite base in the MOCVD equipment according to claim 1 is characterized in that: carry out described boil sour step after, go acid solution on the graphite base with inhaling the article suction that acid wipes acid, carry out described bath step again.
3, the cleaning method of graphite base in the MOCVD equipment according to claim 1, it is characterized in that, describedly boil sour step and comprise: graphite base is put into phosphoric acid boil a period of time, take out the brush graphite base then, part attachment on the graphite base is removed, put into phosphoric acid again and continue to boil.
4, the cleaning method of graphite base in the MOCVD equipment according to claim 1, it is characterized in that: described bath step comprises swinging washes and rinsing step; Wherein swing and wash step and comprise:
The obverse and reverse of graphite base swung wash, with inhaling the article that acid wipes acid graphite base is wiped then, continue again to swing and wash.
5, the cleaning method of graphite base in the MOCVD equipment according to claim 4 is characterized in that, described swinging washed step and comprised:
Earlier successively with front, the back of graphite base, the front is swung and is washed one time again, repeats said process 5 times; With the article of inhaling acid wiping acid graphite base is wiped then; Swing again and wash one time.
6, the cleaning method of the interior graphite base of MOCVD equipment according to claim 4 is characterized in that described rinsing step comprises: will swing washed graphite base and put into the bath groove, and with the hot deionized water flushing, and need taking-up to swing the shampooing suction in the flushing process.
7, according to the cleaning method of graphite base in claim 4 or the 5 described MOCVD equipment, it is characterized in that: describedly inhale that article that acid wipes acid can be that degreasing cotton, chemicals absorption are cotton, in the dust-free paper any.
8, the cleaning method of graphite base in the MOCVD equipment according to claim 1 is characterized in that: described drying steps comprises that elder generation dries up graphite base, toasts again.
9, the cleaning method of graphite base in the MOCVD equipment according to claim 4, it is characterized in that: the described water temperature of washing of swinging is 55 degrees centigrade～65 degrees centigrade, and the water temperature of described flushing is 70 degrees centigrade～100 degrees centigrade.
10, the cleaning method of graphite base in the MOCVD equipment according to claim 1 is characterized in that: the described temperature of acid of boiling is at 80 degrees centigrade～150 degrees centigrade; The temperature of described baking is at 60 degrees centigrade～180 degrees centigrade.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101149154A CN101502835B (en) | 2009-02-09 | 2009-02-09 | Method for cleaning graphite base in MOCVD equipment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101149154A CN101502835B (en) | 2009-02-09 | 2009-02-09 | Method for cleaning graphite base in MOCVD equipment |
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| CN101502835A true CN101502835A (en) | 2009-08-12 |
| CN101502835B CN101502835B (en) | 2011-01-05 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102280396A (en) * | 2011-09-14 | 2011-12-14 | 江阴鑫辉太阳能有限公司 | Graphite boat saturated treating technology |
| CN104998857A (en) * | 2014-04-15 | 2015-10-28 | 宁波宝新不锈钢有限公司 | Dipping repair method of slide way of ABB shape meter slide ring |
| CN112404022A (en) * | 2020-11-20 | 2021-02-26 | 苏州镓港半导体有限公司 | Method for cleaning graphite disc for MOCVD equipment |
| CN114029300A (en) * | 2021-03-12 | 2022-02-11 | 重庆康佳光电技术研究院有限公司 | Method for cleaning graphite plate |
-
2009
- 2009-02-09 CN CN2009101149154A patent/CN101502835B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102280396A (en) * | 2011-09-14 | 2011-12-14 | 江阴鑫辉太阳能有限公司 | Graphite boat saturated treating technology |
| CN104998857A (en) * | 2014-04-15 | 2015-10-28 | 宁波宝新不锈钢有限公司 | Dipping repair method of slide way of ABB shape meter slide ring |
| CN112404022A (en) * | 2020-11-20 | 2021-02-26 | 苏州镓港半导体有限公司 | Method for cleaning graphite disc for MOCVD equipment |
| CN112404022B (en) * | 2020-11-20 | 2022-09-09 | 苏州镓港半导体有限公司 | Method for cleaning graphite disc for MOCVD equipment |
| CN114029300A (en) * | 2021-03-12 | 2022-02-11 | 重庆康佳光电技术研究院有限公司 | Method for cleaning graphite plate |
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| CN101502835B (en) | 2011-01-05 |
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Application publication date: 20090812 Assignee: Crystal energy photoelectric (Changzhou) Co., Ltd. Assignor: Lattice Power (Jiangxi) Co., Ltd. Contract record no.: 2012360000083 Denomination of invention: Method for cleaning graphite base in MOCVD equipment Granted publication date: 20110105 License type: Common License Record date: 20121213 |
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Assignee: LATTICE POWER (CHANGZHOU) Corp. Assignor: LATTICE POWER (JIANGXI) Corp. Contract record no.: 2012360000083 Date of cancellation: 20220228 |