CN106904626A - A kind of preparation method of waterless boron oxide - Google Patents
A kind of preparation method of waterless boron oxide Download PDFInfo
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- CN106904626A CN106904626A CN201510973105.XA CN201510973105A CN106904626A CN 106904626 A CN106904626 A CN 106904626A CN 201510973105 A CN201510973105 A CN 201510973105A CN 106904626 A CN106904626 A CN 106904626A
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- Prior art keywords
- boron oxide
- crucible
- preparation
- purity
- dehydration
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- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910052810 boron oxide Inorganic materials 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 230000018044 dehydration Effects 0.000 claims abstract description 36
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 36
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004327 boric acid Substances 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 208000005156 Dehydration Diseases 0.000 claims description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000000391 smoking effect Effects 0.000 description 3
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/1027—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of preparation method of waterless boron oxide, its step is as follows：(1) vacuum dehydration treatment is carried out to boric acid, obtains boron oxide；(2) boron oxide is placed in crucible, 30min is kept after being heated to 400 ~ 500 DEG C；(3) heating using microwave dewater treatment is carried out to boron oxide, dewatering time is 10 ~ 40min；(4) room temperature is cooled under normal temperature and pressure conditionses of the water content less than 1ppm, obtains waterless boron oxide.Simple production process of the present invention, with low cost into producing, products obtained therefrom water content is in below 150ppm, high purity 99.999%.
Description
Technical Field
The invention relates to the field of boron oxide, in particular to a preparation method of anhydrous high-purity boron oxide.
Background
Boron oxide generally exists in the form of colorless glassy crystals or powder, is the most main oxide of boron, is widely used as a cosolvent in silicate decomposition, a doping agent in the preparation process of semiconductor materials, an acid catalyst in organic synthesis, a refractory additive in the preparation process of paint, the preparation of boron elements and various borides and the like, however, the application of the boron oxide as the auxiliary agent has higher requirements on the water content and the impurity content of boron oxide, for example, in the preparation process of crystals of III-V compound semiconductors such as gallium arsenide, indium phosphide, gallium nitride and the like, anhydrous high-purity boron oxide is required to be used as a liquid sealing agent, the purity of boron oxide is required to be more than or equal to 99.999 percent, and the water content is required to be less than or equal to 150 ppm.
Usually, the normal pressure method or the reduced pressure method is adopted to prepare the boron oxide, but the boron oxide prepared by the method has high water content and more impurities, and the water content and the impurities do not meet the requirements. At present, there is also a preparation method of anhydrous boron oxide, for example, patent No. 200810155689.X, chinese patent with patent name of a preparation method of high temperature covering agent grade boron oxide, the inventive principle is that boron oxide is heated in air, then boron oxide is put into a platinum crucible, and put into a vacuum furnace of medium frequency induction heating at 1500 ℃, and two-stage dehydration process is adopted to dehydrate, so as to obtain boron oxide with water content below 200ppm, however, the preparation method needs higher temperature, the required energy consumption is larger, the requirement for appliances is higher due to overhigh temperature, and the platinum crucible is adopted to contain boron oxide, so the preparation cost is higher, and the method is not beneficial to large-scale production of enterprises.
Disclosure of Invention
The invention aims to provide a preparation method of anhydrous high-purity boron oxide, which has low production cost and simple production process.
In order to solve the problems of the prior art, the invention is realized by the following technical scheme:
a preparation method of anhydrous boron oxide comprises the following steps:
(1) carrying out vacuum dehydration treatment on boric acid to obtain boron oxide;
(2) placing boron oxide in a crucible, heating to 400-500 ℃, and keeping for 30 min;
(3) carrying out microwave heating dehydration treatment on the boron oxide, wherein the dehydration time is 10-40 min;
(4) and cooling to room temperature under the conditions of normal temperature and normal pressure with the water content of less than 1ppm to obtain the anhydrous boron oxide.
The boric acid in the step (1) is high-purity boric acid with the purity of more than or equal to 99.9995 percent.
The vacuum degree of vacuum dehydration in the step (1) is less than 0.1Pa, the temperature is 200-400 ℃, and the time is 30-120 min.
The crucible in the step (2) is a graphite crucible or a glass crucible with a carbon-coated film.
The invention uses high-purity boric acid with the purity of 99.9995 percent as a raw material, dehydrates under the vacuum condition, and simultaneously, the crucible is made of materials which can penetrate through microwaves and resist the temperature of at least 500 ℃, has no pollution to the preparation of boron oxide, and particularly selects a high-purity graphite crucible or a glass crucible with a smoked carbon film, the crucible can not cause boron oxide to be reduced by carbon or react with carbon to generate solid solution under the low-temperature condition, and based on the reasons, the purity of the obtained product is high and can reach more than 99.999 percent, thereby meeting the process requirements of the liquid sealing agent required by the growth of crystals such as gallium arsenide and the like.
The microwave heating dehydration method has the advantages that the microwave heating dehydration is adopted, the dehydration temperature is greatly reduced, the energy consumption is reduced, the requirement on equipment is reduced, and an expensive platinum crucible is not required, so that the production cost is reduced, the benefit of an enterprise is improved, the microwave heating dehydration is adopted, the dehydration time is shortened, the production efficiency is improved, and the product yield is favorably improved.
The invention has simple production process and low production cost, and the obtained product has the water content below 150ppm and the purity as high as 99.999 percent.
Detailed Description
The invention discloses a preparation method of anhydrous high-purity boron oxide, which comprises the following specific steps:
carrying out vacuum dehydration treatment on high-purity boric acid with the purity of more than or equal to 99.9995% in an environment with the temperature of 200-400 ℃ and the vacuum degree of less than 0.1Pa, wherein the dehydration time is 30-120 min, so as to obtain boron oxide; placing boron oxide in a crucible, heating to 400-500 ℃, and keeping for 30min, wherein the crucible is made of a material which can transmit microwave and resist the temperature of at least 500 ℃, preferably a graphite crucible or a carbon smoking film glass crucible, most preferably a high-purity graphite crucible, and is commercially available, and the carbon smoking film glass crucible is obtained by placing the glass crucible in a carbon smoking furnace and depositing a carbon film. The crucible can not cause boron oxide to be reduced by carbon or react with carbon to generate solid solution to cause boron oxide pollution under the condition of low temperature, and can further improve the product purity; the boron oxide is subjected to microwave heating dehydration treatment, the dehydration time is 10-40 min, the microwave frequency and the like are not limited, microwave heating dehydration treatment can be performed by using a microwave oven or a microwave vacuum dryer and the like according to the characteristics of raw materials, and the boron oxide dehydration treatment method has the characteristics of low energy consumption, high efficiency, uniform temperature, small temperature gradient and the like, reduces the production cost, and improves the product quality; and cooling to room temperature under the conditions of normal temperature and normal pressure with the water content of less than 1ppm to obtain the anhydrous boron oxide.
The principle of microwave heating dehydration is that microwave penetrates through the material to enable water molecules in the material to generate directional high-frequency oscillation motion, the water molecules mutually rub to generate heat, a heating body is formed inside and outside the whole material at the same time, so that the water molecules are rapidly heated and separated out, the rapid drying effect is achieved, the dehydration temperature can be greatly reduced by adopting microwave heating dehydration, the energy consumption is reduced, the requirement on equipment is reduced, a platinum crucible with high price is not required to be adopted, the production cost is reduced, the benefit of an enterprise is improved, the dehydration time is shortened by adopting microwave heating dehydration, the production efficiency is improved, and the product yield is favorably improved.
The following are non-limiting examples of the present invention, and the specific parameters may be varied according to the actual circumstances.
Example 1
A preparation method of anhydrous boron oxide comprises the following steps: (1) carrying out vacuum dehydration treatment on high-purity boric acid with the purity of more than or equal to 99.9995% under the conditions that the vacuum degree is less than 0.1Pa and the temperature is 400 ℃, wherein the dehydration time is 120min, and obtaining boron oxide; (2) placing boron oxide in a high-purity graphite crucible, heating to 400 ℃, and keeping for 30 min; (3) placing boron oxide in a microwave oven, and performing microwave heating dehydration treatment for 10 min; (4) and cooling to room temperature under the conditions of normal temperature and normal pressure with the water content of less than 1ppm to obtain the anhydrous boron oxide.
Example 2
A preparation method of anhydrous boron oxide comprises the following steps: (1) carrying out vacuum dehydration treatment on high-purity boric acid with the purity of more than or equal to 99.9995% under the conditions that the vacuum degree is less than 0.1Pa and the temperature is 200 ℃, wherein the dehydration time is 120min, and obtaining boron oxide; (2) placing boron oxide in a glass crucible with a carbon fumigating film, heating to 450 deg.C, and maintaining for 30 min; (3) placing boron oxide in a microwave vacuum dryer and performing microwave heating dehydration treatment on the boron oxide, wherein the dehydration time is 25 min; (4) and cooling to room temperature under the conditions of normal temperature and normal pressure with the water content of less than 1ppm to obtain the anhydrous boron oxide.
Example 3
A preparation method of anhydrous boron oxide comprises the following steps: (1) carrying out vacuum dehydration treatment on high-purity boric acid with the purity of more than or equal to 99.9995% under the conditions that the vacuum degree is less than 0.1Pa and the temperature is 300 ℃, wherein the dehydration time is 60min, and obtaining boron oxide; (2) placing boron oxide in a high-purity graphite crucible, heating to 500 ℃, and keeping for 30 min; (3) placing boron oxide in a microwave oven, and performing microwave heating dehydration treatment for 40 min; (4) and cooling to room temperature under the conditions of normal temperature and normal pressure with the water content of less than 1ppm to obtain the anhydrous boron oxide.
Claims (2)
1. A preparation method of anhydrous boron oxide comprises the following steps:
(1) carrying out vacuum dehydration treatment on boric acid to obtain boron oxide;
(2) placing boron oxide in a crucible, heating to 400-500 ℃, and keeping for 30 min;
(3) carrying out microwave heating dehydration treatment on the boron oxide, wherein the dehydration time is 10-40 min;
(4) cooling to room temperature under normal temperature and pressure with water content less than 1ppm to obtain anhydrous boron oxide; wherein,
the boric acid in the step (1) is high-purity boric acid with the purity of more than or equal to 99.9995 percent; and the vacuum degree of vacuum dehydration in the step (1) is less than 0.1Pa, the temperature is 200-400 ℃, and the time is 30-120 min.
2. The method for producing anhydrous boron oxide according to claim 1, characterized in that: the crucible in the step (2) is a graphite crucible or a glass crucible with a carbon-coated film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510973105.XA CN106904626A (en) | 2015-12-23 | 2015-12-23 | A kind of preparation method of waterless boron oxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510973105.XA CN106904626A (en) | 2015-12-23 | 2015-12-23 | A kind of preparation method of waterless boron oxide |
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| Publication Number | Publication Date |
|---|---|
| CN106904626A true CN106904626A (en) | 2017-06-30 |
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| CN201510973105.XA Pending CN106904626A (en) | 2015-12-23 | 2015-12-23 | A kind of preparation method of waterless boron oxide |
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| CN (1) | CN106904626A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500305A (en) * | 2017-10-12 | 2017-12-22 | 长葛市联发粮食专业合作社 | A kind of preparation method of boron oxide product |
| CN109211712A (en) * | 2018-10-17 | 2019-01-15 | 东旭科技集团有限公司 | The measuring method of boric anhydride moisture content |
-
2015
- 2015-12-23 CN CN201510973105.XA patent/CN106904626A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500305A (en) * | 2017-10-12 | 2017-12-22 | 长葛市联发粮食专业合作社 | A kind of preparation method of boron oxide product |
| CN109211712A (en) * | 2018-10-17 | 2019-01-15 | 东旭科技集团有限公司 | The measuring method of boric anhydride moisture content |
| CN109211712B (en) * | 2018-10-17 | 2021-03-09 | 东旭光电科技股份有限公司 | Method for measuring water content of boric anhydride |
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| Date | Code | Title | Description |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170630 |
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| WD01 | Invention patent application deemed withdrawn after publication |