CN118637919B - Method for preparing ceramic material from boron carbide grinding waste and application of ceramic material - Google Patents
Method for preparing ceramic material from boron carbide grinding waste and application of ceramic material Download PDFInfo
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- CN118637919B CN118637919B CN202411087181.6A CN202411087181A CN118637919B CN 118637919 B CN118637919 B CN 118637919B CN 202411087181 A CN202411087181 A CN 202411087181A CN 118637919 B CN118637919 B CN 118637919B
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- 239000002699 waste material Substances 0.000 title claims abstract description 61
- 238000000227 grinding Methods 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 32
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052580 B4C Inorganic materials 0.000 title claims abstract description 28
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000000919 ceramic Substances 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims description 21
- 238000000498 ball milling Methods 0.000 claims description 20
- 238000002386 leaching Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000007731 hot pressing Methods 0.000 claims description 12
- 229910052594 sapphire Inorganic materials 0.000 claims description 11
- 239000010980 sapphire Substances 0.000 claims description 11
- 238000005498 polishing Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000004570 mortar (masonry) Substances 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 239000004035 construction material Substances 0.000 claims 1
- 238000004064 recycling Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 239000003082 abrasive agent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a method for preparing a ceramic material by grinding waste boron carbide and application thereof, and belongs to the technical field of preparing ceramics by comprehensively utilizing secondary resources. The invention realizes the recycling of waste resources, changes waste into valuable, protects the environment and has high economic value. The ceramic material prepared by sintering has excellent performance, reaches the market standard, has outstanding hardness and toughness, can be applied to the fields of wear-resistant structural materials and the like in the civil field, and can be applied to the fields of bulletproof clothes, bulletproof armor and the like in the military field. And the operation is simple and feasible, the cost is low, and the industrial production is convenient.
Description
Technical Field
The invention belongs to the technical field of ceramics preparation by comprehensively utilizing secondary resources, and particularly relates to a method for preparing ceramics from boron carbide grinding waste and application thereof.
Background
With the gradual maturity of single crystal growth technology and processing technology, sapphire is increasingly popularized in the industries of LED illuminating lamps, mobile phone cameras, screens, medical equipment, environmental protection and the like. When the sapphire is applied in the field, the sapphire is subjected to grinding and polishing so as to meet the flatness requirement of the application. The traditional grinding adopts diamond as an abrasive to grind the sapphire, but the diamond has high price and general grinding effect, the hardness of boron carbide (B 4 C) is between that of the diamond and the sapphire, and the price is relatively low, and the grinding effect is excellent, so that the B 4 C powder is adopted to polish the sapphire wafer in the industry at present. The polishing mode adopts a free polishing mode, and as the polishing time increases, the polishing efficiency and quality of the B 4 C abrasive material can not meet the requirements due to particle breakage, size change and the like, and the batch of abrasive material can be eliminated, so that B 4 C grinding waste is formed. B 4 C grinding waste has the following characteristics: firstly, the particles are fine, the sapphire grinding and polishing belongs to the finishing process of the end stage of the process, the granularity of the used B 4 C grinding material is finer, and the B 4 C particles are further refined due to the mechanical grinding effect; secondly, the abrasive sapphire contains impurities, and enters the B 4 C abrasive, wherein the main component of the sapphire is Al 2O3, so that the main impurity in the B 4 C abrasive waste is Al 2O3.
B 4 C grinding waste is reused as an abrasive, so that the grinding efficiency is low, the surface is easy to scratch, and no effective method is available at present for recycling the grinding waste.
Disclosure of Invention
In order to solve the technical problems, the properties of the B 4 C grinding waste are researched and analyzed, and the B 4 C grinding waste is considered to have high surface energy when the granularity is fine, so that the grinding waste is suitable for sintering, and the Al 2O3 can play a role in assisting in sintering B 4 C under a proper addition amount. Aiming at the characteristics of B 4 C grinding waste, the application adopts ball milling, crushing, mixing and acid leaching to firstly modify the B 4 C grinding waste, and then adopts a hot-pressing sintering method to prepare the B 4 C ceramic material with high hardness and high toughness from the B 4 C grinding waste. The obtained B 4 C ceramic material can be applied to the field of wear-resistant structural materials such as cutters, bearings, nozzles and the like in the civil field, and can be applied to the fields of bulletproof clothes, bulletproof armor and the like in the military field. In the civil field, the cutting capacity of the B 4 C cutter can be improved due to high hardness, and meanwhile, the wear resistance can be improved due to high hardness, so that the tolerance capacity of the B 4 C bearing and the nozzle is improved. The high toughness can reduce the brittle failure probability of B 4 C cutters, bearings and nozzles, so that the cutter is not easy to break and crack, and the service life is prolonged. In the military field, the high hardness can improve the capability of damaging warheads of the B 4 C bulletproof ceramic, weaken penetration capability of bullets, and the high toughness can remarkably improve the capability of resisting multiple bullets of the B 4 C bulletproof ceramic.
The method of the invention prepares the B 4 C grinding waste into the B 4 C ceramic material with high hardness and high toughness, which not only can avoid the environmental pollution problem caused by solid waste accumulation, but also can change waste into valuables, and the waste is recycled, thereby creating higher economic value.
The technical scheme of the invention is as follows:
a method for preparing a boron carbide ceramic material from boron carbide grinding waste comprises the following steps of;
S1, pretreatment: screening or selecting to remove larger impurities in the waste, and grinding the waste in a mortar;
s2, modifying the pretreated waste material in any one of the following modes:
(1) Ball milling treatment is carried out on the pretreated waste material: ball material mass ratio is 3-6:1, ball milling time is 7-12 h, and ball milling rotating speed is 200-450 r/min;
(2) Carrying out traditional acid leaching treatment or microwave acid leaching treatment on the pretreated waste: the acid liquid is one or more of H 2SO4 solution and HCl solution; the temperature of the traditional acid leaching treatment is 90-250 ℃; the microwave acid leaching treatment temperature is 90-240 ℃;
s3, hot pressing and sintering: drying the material obtained in the step S2, and performing hot-pressing sintering;
the mass percentage of the aluminum oxide in the waste is 8-22 wt%. Further, the mass percentage of the aluminum oxide in the waste is 8-13 wt%.
The waste is boron carbide grinding waste for sapphire finish grinding or polishing.
S2, ball milling is carried out by adopting a dry method or a wet method; and ethanol is used as a medium during wet ball milling, and the mass ratio of the ethanol to the pretreated waste is 3.5-6.5:1.
The ball milling in S2 adopts ZrO 2 or B 4 C balls.
The mass concentration of the acid liquor in the S2 is 20% -50%, and the mass ratio mL/g of the acid liquor to the pretreated waste is 3-10:1.
And S2, microwave power of the microwave acid leaching treatment is 20-90 kW.
And S2, the heating rate of the microwave acid leaching treatment is 5-15 ℃/min.
And S3, the hot-pressing sintering process comprises the steps of heating to 1900-2100 ℃ at a speed of 20-30 ℃/min, pressurizing, wherein the pressure is 15-60 MPa, and maintaining the temperature for 10-40 min. Further, after the temperature is raised to 1900-2100 ℃, the pressure is increased to 15-60 MPa at a speed of 3-20 MPa/s.
The invention also provides application of the boron carbide ceramic material obtained by the method in bulletproof clothes and bulletproof armor.
The invention also provides application of the boron carbide ceramic material obtained by the method in a wear-resistant structural material. The wear resistant material includes a cutter, a bearing, and a nozzle.
The invention has the beneficial effects that:
(1) The recycling of waste resources is realized, waste materials are changed into valuable materials, the environment is protected, and the method has high economic value.
(2) The ceramic material prepared by sintering has excellent performance, reaches the market standard, has outstanding hardness and toughness, can be applied to the fields of wear-resistant structural materials and the like in the civil field, and can be applied to the fields of bulletproof clothes, bulletproof armor and the like in the military field.
(3) In the ball milling pretreatment process, the boron carbide ceramic material with high hardness and excellent toughness is obtained under the condition of higher Al 2O3 content. The waste materials are mutually ground materials, grinding can activate powder, the surface energy of the powder is improved, meanwhile, the structural defect of the powder is increased, the powder does not strictly meet the stoichiometric ratio, diffusion and densification are promoted in the sintering process, and the activity of the B 4 C grinding waste materials is higher than that of common powder. Secondly, the process specifically carries out ball milling, crushing and dispersing, further activates powder, breaks up agglomerated B 4 C and Al 2O3, forms smaller particles, and improves uniformity. Under the promotion of both aspects, the hardness and toughness of the ceramic material obtained by sintering are improved compared with those of commercial pure powder, and the toughness is obviously improved.
(4) And (3) carrying out proper acid leaching treatment on the basis of higher activity of the B 4 C grinding waste to form smaller particles, improving the uniformity, and obtaining the boron carbide ceramic material with high hardness and excellent toughness.
(5) The operation is simple and feasible, the cost is low, and the industrial production is convenient.
Detailed Description
The invention will be further described in detail with reference to specific examples in order to make the invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In the embodiment of the invention, a three-point bending method is adopted for bending strength, and an electronic universal mechanical testing machine is adopted.
In the examples of the present invention, the hardness was measured by the Vickers hardness method and a micro Vickers hardness tester was used.
The fracture toughness of the examples of the present invention was measured by indentation.
The composition of the boron carbide mill waste used in this example was B 4C 87.32 wt%、 Al2O3, 10.92, wt% by weight, the other 1.76% by weight, and the median particle size of the waste was 3.3. Mu.m.
Example 1
And (3) taking boron carbide grinding waste 10g, mixing by adopting wet ball milling, and using ZrO 2 balls, wherein the mass ratio of the balls to the materials is 4:1, and the mass ratio of the ethanol to the materials is 4:1. Ball milling time is 10 h, and ball milling rotating speed is 350 r/min. Drying the material in a vacuum oven at 80 ℃ for 4 h, wherein the median particle diameter of the boron carbide grinding waste is 1.85 mu m, then performing hot-pressing sintering, heating to 2000 ℃ at a speed of 30 ℃/min, then pressurizing at 15 MPa/s, maintaining the pressure at 20 MPa, and preserving the heat and the pressure at 30 min. The ceramic obtained was well formed, had a hardness of 32 GPa, a flexural strength of 450 MPa and a fracture toughness of 4.8 MPa.m 1/2.
Example 2
And (3) modifying the boron carbide grinding waste 10 g by adopting a microwave acid leaching method, wherein the mass concentration of H 2SO4 is 35%, the liquid-solid ratio is 6 mL/g, the heating rate is 8 ℃/min, the temperature is 240 ℃, and the power is 50 kW. Drying the materials in a vacuum oven at 80 ℃ for 4 h, wherein the median particle diameter of the boron carbide grinding waste is 1.75 mu m, then performing hot-pressing sintering, heating to 2000 ℃ at a speed of 30 ℃/min, then pressurizing at 15 MPa/s, maintaining the pressure at 20 MPa, and preserving the heat and the pressure at 30 min. The resulting ceramic was well formed, with Al 2O3 remaining approximately 2.5 wt%, a hardness of 29.5 GPa, a flexural strength of 380 MPa, and a fracture toughness of 4.2 MPa m 1/2.
Example 3
And (3) taking the boron carbide grinding waste 10 g, modifying by adopting a conventional acid leaching method, wherein the mass concentration of H 2SO4 is 35%, the liquid-solid ratio is 6 mL/g, the heating rate is 8 ℃/min, and the temperature is 150 ℃. Drying the materials in a vacuum oven at 80 ℃ for 4h, wherein the median particle diameter of the boron carbide grinding waste is 1.98 mu m, then performing hot-pressing sintering, heating to 2000 ℃ at a speed of 30 ℃/min, then pressurizing at 15 MPa/s, maintaining the pressure at 20 MPa, and preserving the heat and the pressure at 30 min. The resulting ceramic was well formed, with Al 2O3 remaining about 7wt%, hardness 30.8 GPa, flexural strength 410 MPa, fracture toughness 4.46MPa m 1/2.
Comparative example 1
Taking the boron carbide grinding waste 10 g, directly performing hot-pressing sintering, heating to 2000 ℃ at a speed of 30 ℃/min, then pressurizing at a pressurizing speed of 15 MPa/s, and maintaining the temperature and pressure of 20MPa and 30 min. The obtained ceramic is rapidly disintegrated under the action of slight external force, and the molding and solidification are not firm.
Comparative example 2
9G of boron carbide (with the median particle size of 1.33 microns) is taken, 2O3 g of Al is added into the boron carbide, the mixture is uniformly mixed, wet ball milling and mixing are adopted, zrO 2 balls are used, the ball mass ratio is 4:1, ethanol is used as a mixing medium, and the mass ratio of ethanol to the material is 4:1. Ball milling time is 10 h, and ball milling rotating speed is 350 r/min. And (3) drying the material, performing hot-pressing sintering, heating to 2000 ℃ at a heating speed of 30 ℃/min, and then pressurizing at a pressurizing speed of 15 MPa/s, wherein the pressure is 20 MPa, and maintaining the temperature and pressure for 30 min. The obtained ceramic has good molding, the toughness is 3.6 MPa.m 1/2, and the hardness is 30.3 GPa.
Claims (7)
1. A method for preparing a ceramic material from boron carbide grinding waste is characterized by comprising the following steps: comprises the following steps of;
S1, pretreatment: screening or selecting to remove larger impurities in the waste, and grinding the waste in a mortar;
s2, modifying the pretreated waste material in any one of the following modes:
(1) Ball milling treatment is carried out on the pretreated waste material: ball material mass ratio is 3-6:1, ball milling time is 7-12 h, and ball milling rotating speed is 200-450 r/min;
(2) Carrying out traditional acid leaching treatment or microwave acid leaching treatment on the pretreated waste: the acid liquid is one or more of H 2SO4 solution and HCl solution; the temperature of the conventional acid leaching treatment is 90-250 ℃; the microwave acid leaching treatment temperature is 90-240 ℃;
s3, hot pressing and sintering: drying the material obtained in the step S2, and performing hot-pressing sintering to obtain boron carbide ceramic;
The mass percentage of the aluminum oxide in the waste is 8-22wt%;
the mass concentration of the acid liquor in the S2 is 20% -50%, and the mass ratio mL/g of the acid liquor to the pretreated waste is 3-10:1;
And S3, the hot-pressing sintering process comprises the steps of heating to 1900-2100 ℃ at a speed of 20-30 ℃/min, pressurizing, wherein the pressure is 15-60 MPa, and maintaining the temperature for 10-40 min.
2. A method for preparing ceramic materials from boron carbide mill waste as claimed in claim 1, wherein: the waste is boron carbide grinding waste for sapphire finish grinding or polishing.
3. A method for preparing ceramic materials from boron carbide mill waste as claimed in claim 1, wherein: s2, ball milling is carried out by adopting a dry method or a wet method; and ethanol is used as a medium during wet ball milling, and the mass ratio of the ethanol to the pretreated waste is 3.5-6.5:1.
4. A method for preparing ceramic materials from boron carbide mill waste as claimed in claim 1, wherein: and S2, microwave power is 20-90 kW.
5. A method for preparing ceramic materials from boron carbide mill waste as claimed in claim 1 or 4, wherein: and S2, the heating rate of the microwave acid leaching treatment is 5-15 ℃/min.
6. Use of the ceramic material obtained by the method of claim 1 in body armor and ballistic armor.
7. Use of a ceramic material obtained by the method of claim 1 in a wear resistant construction material.
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| CN108276003A (en) * | 2018-02-13 | 2018-07-13 | 苏州纳朴材料科技有限公司 | A method of preparing boron carbide complex phase ceramic using sapphire grinding dead meal |
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| JP5057327B2 (en) * | 2007-09-14 | 2012-10-24 | 学校法人同志社 | Boron carbide ceramics and method for producing the same |
| CN102731093A (en) * | 2011-04-06 | 2012-10-17 | 鲁东大学 | Method for low-temperature densification sintering of boron carbide-based ceramic material |
| CN107986284A (en) * | 2017-12-08 | 2018-05-04 | 中国科学院青海盐湖研究所 | It is a kind of that the method that boron carbide is recycled in waste material is ground from sapphire |
| CN107902659B (en) * | 2017-12-08 | 2021-11-26 | 中国科学院青海盐湖研究所 | Method for recovering and purifying boron carbide from sapphire grinding waste |
| KR102364295B1 (en) * | 2020-02-28 | 2022-02-21 | 한국과학기술연구원 | Boron carbide composite and its fabrication method |
| CN117263691A (en) * | 2023-09-15 | 2023-12-22 | 中国科学院金属研究所 | B (B) 4 Preparation method of C composite ceramic material |
| CN117945761B (en) * | 2024-03-27 | 2024-06-18 | 东北大学 | Method for preparing ceramic material from boron carbide dust collection waste |
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| CN108276003A (en) * | 2018-02-13 | 2018-07-13 | 苏州纳朴材料科技有限公司 | A method of preparing boron carbide complex phase ceramic using sapphire grinding dead meal |
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