CN1250347C - Chemical washing method of boron nitride crucible - Google Patents
Chemical washing method of boron nitride crucible Download PDFInfo
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- CN1250347C CN1250347C CN 03110866 CN03110866A CN1250347C CN 1250347 C CN1250347 C CN 1250347C CN 03110866 CN03110866 CN 03110866 CN 03110866 A CN03110866 A CN 03110866A CN 1250347 C CN1250347 C CN 1250347C
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- boron nitride
- nitride crucible
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Abstract
The present invention relates to a chemical washing method for boron nitride crucibles, which belongs to the field of chemical washing. Mixed acid liquor prepared from concentrated sulfuric acid, concentrated nitric acid and hydrofluoric acid and NaOH solution with the concentration of 60% are utilized to strip infiltrated corrosion on the surface layer of a boron nitride crucible, and the integrity of the boron nitride crucible can be guaranteed. The boron nitride crucible can be thoroughly washed without any residue impurity, and the boron nitride crucible can be used for multiple times to melt different materials, so that the cost is reduced.
Description
Technical field: the invention belongs to the Chemical cleaning field, relate to the chemical cleaning method of boron nitride crucible.
Background technology: boron nitride is a kind of pure white lubricity good heat-resistance crystal, nearly 3000 degrees centigrade of fusing point; Its insulating properties are good especially, and at high temperature, its insulating properties surpass any resistant to elevated temperatures oxide, have good conductivity of heat simultaneously again; Chemical property is stable, and nearly all motlten metal all is chemical inertness, and inorganic acid and chemical reagent are also all had corrosion resistance.Because height chemical stability, heat endurance, the insulating properties of boron nitride and be again the good conductor of heat make it be made into the crucible of a lot of materials of fusion.But boron nitride crucible is through after using for a long time, the material of fusion can soak into its top layer, conventional method is difficult to it is cleaned up, and cause a kind of highly purified material of maintenance that needs of every fusion just to need a new boron nitride crucible, and boron nitride crucible is all very expensive always.
Summary of the invention: the repeated using method that the purpose of this invention is to provide a kind of boron nitride crucible, just providing a kind of chemical method simple and easy to do, with low cost specifically thoroughly cleans used boron nitride crucible, not residual any impurity, as before pure white, same crucible can repeatedly be used, the material that fusion is different reduces cost.
For achieving the above object, the concrete cleaning step to boron nitride crucible is as follows among the present invention:
1. select corresponding chemical reagent that boron nitride crucible is tentatively cleaned according to the residual original melted material of boron nitride crucible.
2. using volume ratio is that 1: 1: 1 the concentrated sulfuric acid, red fuming nitric acid (RFNA), the mix acid liquor etch of hydrofluoric acid configuration were handled more than 15 minutes, uses deionized water rinsing then.
3. boil more than 30 minutes with 60% caustic soda (NaOH) solution, use deionized water rinsing then, use the ultrasonic processing twice of deionized water again, each more than 10 minutes.
4. be that 1: 3 red fuming nitric acid (RFNA), concentrated hydrochloric acid mix acid liquor (chloroazotic acid) boils with volume ratio,, use the ultrasonic processing twice of deionized water again until making this mix acid liquor again after the yellowing, use deionized water rinsing by the golden yellow redness that becomes, each more than 10 minutes.
5. the deionization poach is three times, and is each more than 15 minutes, then with the infrared lamp oven dry, puts into the logical oxygen baking of high temperature dispersing furnace more than 12 hours.
Finish after above-mentioned 5 steps, boron nitride crucible can thoroughly clean up.
Good effect of the present invention: be that 1: 1: 1 mix acid liquor of the concentrated sulfuric acid, red fuming nitric acid (RFNA), hydrofluoric acid configuration and top layer corrosion that 60% caustic soda (NaOH) solution is soaked into boron nitride crucible are peeled off and can be guaranteed the complete of boron nitride crucible with volume ratio, boron nitride crucible thoroughly can be cleaned up, not residual any impurity, it can repeatedly be used, the material that fusion is different reduces cost.
The specific embodiment:
The specific embodiment 1:
The Chemical cleaning of remaining silicon (Si) in the boron nitride crucible
1. use 48% hydrofluoric acid solution,, use deionized water rinsing then remaining silicon (Si) dissolving.
2. using volume ratio is that 1: 1: 1 the concentrated sulfuric acid, red fuming nitric acid (RFNA), the mix acid liquor etch of hydrofluoric acid configuration were handled 15 minutes, uses deionized water rinsing then.
3. boiled 30 minutes with 60% caustic soda (NaOH) solution, use deionized water rinsing then, use the ultrasonic processing twice of deionized water again, each 10 minutes.
4. be that 1: 3 red fuming nitric acid (RFNA), concentrated hydrochloric acid mix acid liquor (chloroazotic acid) boils with volume ratio, make this mix acid liquor again till the yellowing, use deionized water rinsing then, use the ultrasonic processing twice of deionized water again, each 10 minutes by the golden yellow redness that becomes.
5. the deionization poach is three times, each 15 minutes, then with the infrared lamp oven dry, puts into the logical oxygen baking of high temperature dispersing furnace 12 hours.
The specific embodiment 2:
Original remaining manganese metal (Mn) in the boron nitride crucible
1. use 10% salpeter solution,, use deionized water rinsing then remaining manganese metal (Mn) dissolving.
2. using volume ratio is that 1: 1: 1 the concentrated sulfuric acid, red fuming nitric acid (RFNA), the mix acid liquor etch of hydrofluoric acid configuration were handled 15 minutes, uses deionized water rinsing then.
3. boiled 30 minutes with 60% caustic soda (NaOH) solution, use deionized water rinsing then, use the ultrasonic processing twice of deionized water again, each 10 minutes.
4. be that 1: 3 nitric acid, mixed in hydrochloric acid acid solution boiled with volume ratio, again till the yellowing, use deionized water rinsing by the golden yellow redness that becomes then, use the ultrasonic processing twice of deionized water again, each 10 minutes until this mix acid liquor.
5. the deionization poach is three times, each 15 minutes, then with the infrared lamp oven dry, puts into the logical oxygen baking of high temperature dispersing furnace 12 hours.
According to above two specific embodiment steps just boron nitride crucible thoroughly clean up, crucible is placed in the vacuum chamber 1400 degrees centigrade of bakings after, utilize QMS to detect less than impurity.
Claims (3)
1, a kind of chemical cleaning method of boron nitride crucible adopts chemistry and ultrasonic processing method that boron nitride crucible is thoroughly cleaned, and it is characterized in that adopting following steps:
A. select corresponding chemical reagent that boron nitride crucible is tentatively cleaned according to the residual original melted material of boron nitride crucible;
B. using volume ratio is that 1: 1: 1 the concentrated sulfuric acid, red fuming nitric acid (RFNA), the mix acid liquor etch of hydrofluoric acid configuration were handled 15 minutes, uses deionized water rinsing;
C. boiled 30 minutes for 60%NaOH solution with weight percent concentration, use deionized water rinsing, use the ultrasonic processing twice of deionized water again, each 10 minutes;
D. be that 1: 3 red fuming nitric acid (RFNA), concentrated hydrochloric acid mix acid liquor boils with volume ratio,, use the ultrasonic processing twice of deionized water again, each 10 minutes until making this mix acid liquor again after the yellowing, use deionized water rinsing by the golden yellow redness that becomes;
C. the deionization poach is three times, each 15 minutes, then with the infrared lamp oven dry, puts into the logical oxygen baking of high temperature dispersing furnace 12 hours.
2, the chemical cleaning method of a kind of boron nitride crucible according to claim 1 is characterized in that when original melted material residual in the boron nitride crucible is silicon, is that 48% hydrofluoric acid solution tentatively cleans with concentration of volume percent.
3, the chemical cleaning method of a kind of boron nitride crucible according to claim 1 is characterized in that when original melted material residual in the boron nitride crucible is manganese, is that 10% salpeter solution tentatively cleans with concentration of volume percent.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03110866 CN1250347C (en) | 2003-01-13 | 2003-01-13 | Chemical washing method of boron nitride crucible |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 03110866 CN1250347C (en) | 2003-01-13 | 2003-01-13 | Chemical washing method of boron nitride crucible |
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| CN1517159A CN1517159A (en) | 2004-08-04 |
| CN1250347C true CN1250347C (en) | 2006-04-12 |
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| CN 03110866 Expired - Fee Related CN1250347C (en) | 2003-01-13 | 2003-01-13 | Chemical washing method of boron nitride crucible |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102654358A (en) * | 2012-04-24 | 2012-09-05 | 包头稀土研究院 | Aerobic furnace washing method for vacuum smelting furnace |
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| CN101906632B (en) * | 2010-07-06 | 2011-12-07 | 中南钻石股份有限公司 | Method for washing anode bag for electrolyzing synthetic diamonds |
| CN102430552A (en) * | 2011-11-28 | 2012-05-02 | 天通控股股份有限公司 | Cleaning method for crucible for crystal growth |
| CN104368566B (en) * | 2013-08-14 | 2017-08-25 | 台山市华兴光电科技有限公司 | indium phosphide growth crucible cleaning method |
| CN105177708A (en) * | 2015-07-27 | 2015-12-23 | 奥特斯维能源（太仓）有限公司 | Purification method for crucible used for polycrystalline cast ingot |
| CN105887195A (en) * | 2016-06-20 | 2016-08-24 | 云南中科鑫圆晶体材料有限公司 | Pre-cleaning method for using VGF (vertical gradient freeze) method to grow germanium monocrystals |
| CN108057681B (en) * | 2017-10-30 | 2020-10-23 | 武汉金发科技有限公司 | Cleaning method of aluminum oxide crucible of thermal weightlessness instrument |
| CN109530365A (en) * | 2018-11-26 | 2019-03-29 | 中国电子科技集团公司第十研究所 | Molecular beam epitaxy boron nitride crucible cleaning method |
| CN111893555B (en) * | 2020-07-22 | 2021-09-14 | 威科赛乐微电子股份有限公司 | Single crystal PBN crucible treatment process |
| CN112718692A (en) * | 2020-12-09 | 2021-04-30 | 四川富乐德科技发展有限公司 | Method for cleaning LiF crystal of OLED crucible part |
| CN114130753A (en) * | 2021-11-24 | 2022-03-04 | 枣庄睿诺电子科技有限公司 | Process method for removing organic material residues in crucible |
-
2003
- 2003-01-13 CN CN 03110866 patent/CN1250347C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102654358A (en) * | 2012-04-24 | 2012-09-05 | 包头稀土研究院 | Aerobic furnace washing method for vacuum smelting furnace |
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