CN116924811B - Process for producing high-purity silicon hexaboride by one-step method - Google Patents
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- ZRBFEDMQRDRUDG-UHFFFAOYSA-N silicon hexaboride Chemical compound B12B3[Si]45B3B2B4B51 ZRBFEDMQRDRUDG-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 38
- 230000008569 process Effects 0.000 title claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 19
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 17
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 16
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000853 adhesive Substances 0.000 claims abstract description 7
- 230000001070 adhesive effect Effects 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 6
- 239000010439 graphite Substances 0.000 claims abstract description 6
- 239000003921 oil Substances 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 238000009707 resistance sintering Methods 0.000 claims abstract description 6
- 229910052796 boron Inorganic materials 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 238000011068 loading method Methods 0.000 claims description 7
- -1 boron anhydride Chemical class 0.000 claims description 5
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000010304 firing Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 9
- 239000002245 particle Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 239000011863 silicon-based powder Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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Abstract
A process for preparing high-purity silicon hexaboride by a one-step method comprises the steps of taking silicon dioxide, boric anhydride, boron carbide and graphite powder as raw material powder, adding adhesive and magnesium powder, mixing materials in a vacuum ball mill, and pressing into cylindrical blocks by a 400t oil press; and (3) placing the cylindrical block into a graphite crucible of a vacuum resistance sintering furnace, vacuumizing to 0-5Pa, starting to heat, heating to 130kw/h, starting to react when the temperature is increased to 1200 ℃, continuing vacuumizing, continuing to keep the temperature for 2 hours after the vacuum degree is reduced to 3Pa-5Pa, and cooling along with the furnace after power failure to obtain the high-purity silicon hexaboride. The advantages are that: the silicon dioxide, the boric anhydride, the boron carbide and the graphite powder are used as raw materials, the cost of raw materials is low, the high-cost production process of simple substance synthesis is eliminated, the raw materials are pressed into blocks and then are subjected to vacuum firing, the process is completed in one step, the process condition is simple and controllable, the production cost is low, and the obtained silicon hexaboride product has high purity and is suitable for industrial production.
Description
Technical Field
The invention relates to a process for producing high-purity silicon hexaboride by a one-step method.
Background
Silicon hexaboride is one of materials in boron-rich compound ceramics, has high hardness characteristic of the boron-rich compound ceramics, has excellent electrical properties, and is widely applied to the fields of microwave devices, flat panel displays and vacuum wiener devices. Silicon hexaboride has been used in the aerospace and military fields, such as silicon hexaboride for a surface heat-resistant composite coating of hypersonic aircraft, which can accelerate the surface heat dissipation of the hypersonic aircraft.
At present, the preparation method of the silicon hexaboride mainly comprises a vapor deposition method and a simple boron and simple silicon sintering method. The vapor deposition method has complicated operation steps, high pollution risk of production raw materials and is not suitable for industrial production. The simple substance sintering method is characterized in that the price of a raw material boron simple substance is high; CN 106082250a discloses a "method for preparing silicon hexaboride powder", which comprises the following steps: weighing silicon powder with average particle size less than 10 μm and boron powder with average particle size less than 20 μm according to a proportion, ball milling, mixing uniformly, loading into a ceramic crucible, loading into a synthesis furnace, introducing argon gas and dripping SiCl 4 Heating to 1500-1600 ℃, cooling and ball milling to obtain the required SiB 6 And (3) powder. The method can prepare single-phase SiB with high chemical purity and pure phase 6 And (3) powder. However, the elemental boron powder is used as the raw material, the production cost is high, and the fineness requirements on the raw material silicon powder and boron powder are high.
In order to reduce the cost of raw materials, CN112125315A discloses a low-cost high-purity silicon hexaboride production process, which takes diboron trioxide and potassium borohydride as raw materials, obtains boron powder through reduction, and produces high-purity silicon hexaboride with additional raw material silicon powder through a self-propagating method. Has the advantages of low cost of raw materials, energy conservation and high purity of products. However, the process is cost-reducing, boron powder is prepared by reducing diboron trioxide and potassium borohydride, and then high-purity silicon hexaboride is prepared by reacting with silicon powder, and the process is relatively complicated and is completed in two steps.
Disclosure of Invention
The invention aims to solve the technical problem of providing a process for producing high-purity silicon hexaboride by a one-step method, which is simple and controllable, is synthesized by a one-step method, has low production cost, and the obtained silicon hexaboride product has high purity and can be produced in a large scale in an industrialized manner.
The technical scheme of the invention is as follows:
a process for producing high-purity silicon hexaboride by a one-step method comprises the following specific steps:
(1) Mixing material
Taking silicon dioxide, boron anhydride, boron carbide and graphite powder as raw material powder, wherein the molar ratio of the silicon dioxide to the boron anhydride is 1 (1-3), the molar ratio of the silicon dioxide to the boron carbide is 1:1, the molar ratio of the silicon dioxide to the graphite powder is 1 (4-6), adding adhesive and magnesium powder, putting into a 10L vacuum ball mill, and mixing for 2-4 hours to obtain a mixed material;
(2) Briquetting machine
Weighing the mixed materials according to 0.8kg of each part, and pressing the mixed materials into cylindrical blocks by using a 400t oil press;
(3) Preparation of high purity silicon hexaboride
Loading the cylindrical block pressed in the step (2) into a graphite crucible of a vacuum resistance sintering furnace, vacuumizing to 0-5Pa, starting to heat, heating to 130kw/h, heating to 1200 ℃, starting to react, continuously vacuumizing, continuously preserving heat for 2 hours after the vacuum degree is reduced to 3Pa-5Pa, and cooling along with the furnace after power failure to obtain high-purity silicon hexaboride (SiB) 6 )。
Further, the purity of the silicon dioxide powder is 99.9%, the purity of the boron anhydride is 99.8%, the purity of the boron carbide is 99.5%, and the purity of the graphite powder is 99.99%.
Further, the particle size of the silicon dioxide is 600 meshes, the particle size of the boric anhydride is 800 meshes, the particle size of the boron carbide is 400 meshes, and the particle size of the graphite powder is 800 meshes.
Further, the added binder was carboxymethyl cellulose, and 3g of carboxymethyl cellulose was added per 1kg of raw material powder.
Further, 10g of magnesium powder was added per 1kg of the raw material powder.
Further, the charging amount is 3kg-5kg each time when ball milling is carried out in a vacuum ball mill.
The invention has the beneficial effects that:
the silicon dioxide, the boric anhydride, the boron carbide and the graphite powder are used as raw materials, the cost of raw materials is low, the high-cost production process of simple substance synthesis is eliminated, the raw materials are pressed into blocks and then are subjected to vacuum firing, the process is completed in one step, the process condition is simple and controllable, the production cost is low, and the obtained silicon hexaboride product has high purity and can be industrially produced.
Drawings
FIG. 1 is a view of a silicon hexaboride electron microscope image produced in accordance with the present invention;
FIG. 2 is an X-ray diffraction pattern of silicon hexaboride produced in accordance with the present invention.
Detailed Description
The present invention will be explained in more detail by the following examples, which are not intended to limit the scope of the invention.
Example 1
The purity of the silicon dioxide powder is 99.9 percent, the granularity is 600 meshes,
the purity of the boric anhydride is 99.8 percent, the granularity is 800 meshes,
the purity of the boron carbide is 99.5 percent, the granularity is 400 meshes,
the purity of the graphite powder is 99.99 percent, and the granularity is 800 meshes.
(1) Mixing: weighing 4.81kg of silicon dioxide, 16.71kg of boric anhydride, 4.42kg of boron carbide and 5.76kg of graphite powder (the molar ratio is 1:3:1:6), adding 95g of adhesive and 317g of magnesium powder, putting into a 10L vacuum ball mill, charging 5kg each time, and mixing for 3 hours to obtain a mixed material;
(2) And (3) briquetting: weighing 0.8kg of the mixed materials, and pressing the mixed materials into cylindrical blocks by using a 400t oil press;
(3) Preparing high-purity silicon hexaboride: loading the cylindrical block pressed in the step (2) into a graphite crucible of a vacuum resistance sintering furnace, vacuumizing to 3Pa, heating to 130kw/h, reacting at 1200 ℃, observing an internal pressure meter and a vacuum degree meter of the furnace, accelerating the operation of a vacuum pump to discharge a large amount of generated gas when the numerical fluctuation is large, reducing the vacuum degree to 3Pa, continuously preserving heat for 2 hours, and cooling along with the furnace after power failure to obtain high-purity silicon hexaboride (SiB) 6 ) The purity of the high-purity silicon hexaboride is 99.69 percent through detection.
Example 2
The purity of the silicon dioxide powder is 99.9 percent, the granularity is 600 meshes,
the purity of the boric anhydride is 99.8 percent, the granularity is 800 meshes,
the purity of the boron carbide is 99.5 percent, the granularity is 400 meshes,
the purity of the graphite powder is 99.99 percent, and the granularity is 800 meshes.
(1) Mixing: weighing 4.81kg of silicon dioxide, 11.14kg of boric anhydride, 4.42kg of boron carbide and 4.8kg of graphite powder (the molar ratio is 1:2:1:5), adding 75.5g of adhesive and 251.7g of magnesium powder, putting into a 10L vacuum ball mill, charging 4kg each time, and mixing for 2 hours to obtain a mixed material;
(2) And (3) briquetting: weighing 0.8kg of the mixed materials, and pressing the mixed materials into cylindrical blocks by using a 400t oil press;
(3) Preparing high-purity silicon hexaboride: loading the cylindrical block pressed in the step (2) into a graphite crucible of a vacuum resistance sintering furnace, vacuumizing to 4Pa, starting heating, heating to 130kw/h, starting reaction when the temperature is up to 1200 ℃, observing an internal pressure meter and a vacuum degree meter of the furnace, accelerating the operation of a vacuum pump to discharge a large amount of generated gas when the numerical fluctuation is large, reducing the vacuum degree to 4Pa, continuously preserving heat for 2 hours, and cooling along with the furnace after power failure to obtain high-purity silicon hexaboride (SiB) 6 ) The purity of the high-purity silicon hexaboride is 99.61 percent through detection.
Example 3
The purity of the silicon dioxide powder is 99.9 percent, the granularity is 600 meshes,
the purity of the boric anhydride is 99.8 percent, the granularity is 800 meshes,
the purity of the boron carbide is 99.5 percent, the granularity is 400 meshes,
the purity of the graphite powder is 99.99 percent, and the granularity is 800 meshes.
(1) Mixing: weighing 4.81kg of silicon dioxide, 5.57kg of boric anhydride, 4.42kg of boron carbide and 3.84kg of graphite powder (the molar ratio is 1:1:1:4), adding 56g of adhesive and 18.64g of magnesium powder, putting into a 10L vacuum ball mill, charging 3kg each time, and mixing for 4 hours to obtain a mixed material;
(2) And (3) briquetting: weighing 0.8kg of the mixed materials, and pressing the mixed materials into cylindrical blocks by using a 400t oil press;
(3) Preparing high-purity silicon hexaboride: loading the cylindrical block pressed in the step (2) into a graphite crucible of a vacuum resistance sintering furnace, vacuumizing to 5Pa, starting heating, heating to 130kw/h, starting reaction when the temperature is up to 1200 ℃, observing an internal pressure meter and a vacuum degree meter of the furnace, accelerating the operation of a vacuum pump to discharge a large amount of generated gas when the numerical fluctuation is large, reducing the vacuum degree to 5Pa, continuously preserving heat for 2 hours, and cooling along with the furnace after power failure to obtain high-purity silicon hexaboride (SiB) 6 ) The purity of the high-purity silicon hexaboride is 99.55 percent through detection.
The above is only a specific embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A process for producing high-purity silicon hexaboride by a one-step method is characterized in that,
the method comprises the following specific steps:
(1) Mixing material
Taking silicon dioxide, boron anhydride, boron carbide and graphite powder as raw material powder, wherein the molar ratio of the silicon dioxide to the boron anhydride is 1 (1-3), the molar ratio of the silicon dioxide to the boron carbide is 1:1, the molar ratio of the silicon dioxide to the graphite powder is 1 (4-6), adding adhesive and magnesium powder, putting into a 10L vacuum ball mill, and mixing for 2-4 hours to obtain a mixed material;
(2) Briquetting machine
Weighing the mixed materials according to 0.8kg of each part, and pressing the mixed materials into cylindrical blocks by using a 400t oil press;
(3) Preparation of high purity silicon hexaboride
And (3) loading the cylindrical block pressed in the step (2) into a graphite crucible of a vacuum resistance sintering furnace, vacuumizing to 0-5Pa, starting to heat, wherein the heating power is 130kw/h, the temperature is increased to 1200 ℃, starting to react, continuously vacuumizing, continuously preserving heat for 2 hours after the vacuum degree is reduced to 3Pa-5Pa, and cooling along with the furnace after power failure to obtain the high-purity silicon hexaboride.
2. The process for producing high purity silicon hexaboride by the one-step method according to claim 1, characterized in that: the purity of the silicon dioxide powder is 99.9%, the purity of the boric anhydride is 99.8%, the purity of the boron carbide is 99.5%, and the purity of the graphite powder is 99.99%.
3. The process for producing high purity silicon hexaboride by the one-step method according to claim 1, characterized in that: the granularity of the silicon dioxide is 600 meshes, the granularity of the boric anhydride is 800 meshes, the granularity of the boron carbide is 400 meshes, and the granularity of the graphite powder is 800 meshes.
4. The process for producing high purity silicon hexaboride by the one-step method according to claim 1, characterized in that: the added adhesive is carboxymethyl cellulose, and 3g of carboxymethyl cellulose is added to 1kg of raw material powder.
5. The process for producing high purity silicon hexaboride by the one-step method according to claim 1, characterized in that: 10g of magnesium powder is added into each 1kg of raw material powder.
6. The process for producing high purity silicon hexaboride by the one-step method according to claim 1, characterized in that: the charging amount is 3kg-5kg each time when ball milling is carried out in a vacuum ball mill.
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Citations (6)
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| GB860328A (en) * | 1958-03-13 | 1961-02-01 | Kanthal Ab | Improvements in or relating to sintered bodies being resistant to heat, oxidation and |
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| UA65125A (en) * | 2003-06-05 | 2004-03-15 | V M Bakul Inst Of Super Hard M | A method for preparing the silicon hexaboride sib6 ceramics |
| CN106082250A (en) * | 2016-07-07 | 2016-11-09 | 福斯曼科技（北京）有限公司 | A kind of high-purity silicon hexaboride powder preparation method |
| CN112125315A (en) * | 2020-09-25 | 2020-12-25 | 辽宁中色新材科技有限公司 | Low-cost high-purity silicon hexaboride production process |
| CN114409412A (en) * | 2020-10-28 | 2022-04-29 | 中国科学院理化技术研究所 | SiB6Chemical furnace synthesis method |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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