技术领域technical field
本发明属于晶体回收料制备工艺技术领域,尤其涉及一种蓝宝石晶体回收料制备方法。The invention belongs to the technical field of preparation technology of reclaimed crystal materials, and in particular relates to a method for preparing reclaimed sapphire crystal materials.
背景技术Background technique
蓝宝石单晶作为一种优良透波材料,在紫外、可见光、红外波段、微波都具有良好的透波率,可以满足多模式复合制导(电视、红外成像、雷达等)的要求;同时蓝宝石单晶具有优良的机械性能、化学稳定性,耐高温性能好,强度高、硬度大,可以同时满足超高音速导弹对透波材料的苛刻要求。在材料的制备工艺方面蓝宝石可以生长单晶,然后加工成型,成品性能与单晶性能相同,而其它材料主要利用粉末热压铸烧结成型,其在性能上比原来的要稍低。因此,蓝宝石单晶已成为先进国家高速战斗机、导弹等中波透红外窗口材料的极佳选择。As an excellent wave-transparent material, sapphire single crystal has good wave transmittance in ultraviolet, visible light, infrared bands, and microwaves, which can meet the requirements of multi-mode composite guidance (television, infrared imaging, radar, etc.); at the same time, sapphire single crystal It has excellent mechanical properties, chemical stability, good high temperature resistance, high strength and high hardness, and can meet the stringent requirements of hypersonic missiles for wave-transparent materials at the same time. In terms of material preparation process, sapphire can grow single crystal, and then process it into shape. The performance of the finished product is the same as that of single crystal, while other materials are mainly formed by powder hot pressing and sintering, and their performance is slightly lower than the original one. Therefore, sapphire single crystal has become an excellent choice for advanced countries' high-speed fighter jets, missiles and other medium-wave infrared-transmitting window materials.
蓝宝石晶体生长需要用到70%的高纯度块状回收料。目前蓝宝石晶体生长需要的块状回收料主要依靠铁锤敲碎,蓝宝石晶体莫氏硬度达到9,铁锤击打很困难;同时,残留在蓝宝石颗粒表面的铁离子难以清洗干净,影响回收料的纯度,造成生长出的蓝宝石晶体利用率低。Sapphire crystal growth requires the use of 70% high-purity bulk recycled materials. At present, the bulk recycled materials required for the growth of sapphire crystals are mainly broken by hammers. The Mohs hardness of sapphire crystals reaches 9, and it is very difficult to hit them with hammers. At the same time, the iron ions remaining on the surface of sapphire particles are difficult to clean, which affects the quality of recycled materials. Purity, resulting in low utilization rate of grown sapphire crystals.
发明内容Contents of the invention
为解决上述技术问题,本发明提供一种不对回收料产生二次污染的蓝宝石晶体回收料制备方法。In order to solve the above-mentioned technical problems, the present invention provides a method for preparing sapphire crystal recycled materials that does not cause secondary pollution to the recycled materials.
本发明的目的通过下述技术方案来实现:The purpose of the present invention is achieved through the following technical solutions:
(1)将大尺寸蓝宝石晶体回收料放入清洗机内,加热至80℃,保温1小时,进行脱胶处理;(1) Put the recycled large-size sapphire crystal into the cleaning machine, heat it to 80°C, keep it warm for 1 hour, and carry out degumming treatment;
(2)脱胶后的蓝宝石晶体放入超声波清洗机内,用强度为50W/cm2超声波清洗1.5小时;(2) Put the degummed sapphire crystal into an ultrasonic cleaning machine and clean it with an ultrasonic wave with a strength of 50W/cm2 for 1.5 hours;
(3)清洗干净的蓝宝石晶体装入铝箱,放入马弗炉内加热至400℃,保温1.5小时;(3) Put the cleaned sapphire crystal into an aluminum box, heat it in a muffle furnace to 400°C, and keep it warm for 1.5 hours;
(4)取出盛有蓝宝石晶体的铝箱,用大量的RO水(通过反渗透技术制作而成的水)冲洗蓝宝石晶体15分钟;(4) Take out the aluminum box containing the sapphire crystal, and rinse the sapphire crystal with a large amount of RO water (water produced by reverse osmosis technology) for 15 minutes;
(5)用铝锤粉碎蓝宝石晶体;(5) Crush the sapphire crystal with an aluminum hammer;
(6)用RO水清洗粉碎后的蓝宝石颗粒20分钟;(6) Wash the crushed sapphire particles with RO water for 20 minutes;
(7)蓝宝石颗粒装入铝盘内放入烘箱,烘箱温度调到200℃,烘干1.5小时;(7) Put the sapphire particles into an aluminum tray and put them in an oven, adjust the temperature of the oven to 200°C, and dry for 1.5 hours;
(8)烘干后的蓝宝石颗粒降至室温即可进行包装、贮藏。(8) After drying, the sapphire particles can be packaged and stored after cooling down to room temperature.
采用本发明方法,避免了铁锤与蓝宝石晶体的直接接触,杜绝对回收料的二次污染,从而提高了回收料的纯度。By adopting the method of the invention, the direct contact between the iron hammer and the sapphire crystal is avoided, and the secondary pollution to the reclaimed material is prevented, thereby improving the purity of the reclaimed material.
作为本发明进一步的改进,在上述步骤(5)中,将蓝宝石晶体粉碎为10毫米的颗粒,确保回收料粒度均匀。As a further improvement of the present invention, in the above step (5), the sapphire crystal is crushed into particles of 10 mm to ensure that the particle size of the recycled material is uniform.
具体实施方式Detailed ways
下面通过具体的实施例对本发明作进一步的说明。The present invention will be further described below by specific examples.
将大尺寸蓝宝石晶体回收料约80kg放入清洗机内,加热至80℃,保温1小时,进行脱胶处理;脱胶后的蓝宝石晶体放入超声波清洗机内,用强度为50W/cm2超声波清洗1.5小时;清洗干净的蓝宝石晶体装入铝箱,放入马弗炉内加热至400℃,保温1.5小时;取出盛有蓝宝石晶体的铝箱,用大量的RO水(通过反渗透技术制作而成的水)冲洗蓝宝石晶体15分钟;用铝锤粉碎蓝宝石晶体;将蓝宝石晶体粉碎为10毫米的颗粒为优选方案,确保回收料粒度均匀;用RO水清洗粉碎后的蓝宝石颗粒20分钟;蓝宝石颗粒装入铝盘内放入烘箱,烘箱温度调到200℃,烘干1.5小时;烘干后的蓝宝石颗粒降至室温即可进行包装、贮藏。Put about 80kg of large-sized sapphire crystal reclaimed materials into the cleaning machine, heat to 80°C, keep warm for 1 hour, and perform degumming treatment; put the degummed sapphire crystal into the ultrasonic cleaning machine, and use ultrasonic cleaning with a strength of 50W/cm2 for 1.5 hours ; Put the cleaned sapphire crystal into an aluminum box, heat it in a muffle furnace to 400°C, and keep it warm for 1.5 hours; take out the aluminum box containing the sapphire crystal, and use a large amount of RO water (water made by reverse osmosis technology) ) to wash the sapphire crystal for 15 minutes; crush the sapphire crystal with an aluminum hammer; crush the sapphire crystal into 10 mm particles to ensure uniform particle size of the recycled material; wash the crushed sapphire particles with RO water for 20 minutes; put the sapphire particles into aluminum Put the tray into an oven, adjust the oven temperature to 200°C, and dry for 1.5 hours; the dried sapphire particles can be packaged and stored after cooling down to room temperature.
以上实施例的描述较为具体、详细,但并不能因此而理解为对本专利范围的限制,应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。The description of the above embodiments is relatively specific and detailed, but it should not be interpreted as limiting the scope of this patent. Several modifications and improvements are made, all of which belong to the protection scope of the present invention.
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210407595.3ACN103011897B (en) | 2012-10-24 | 2012-10-24 | Preparation method of sapphire crystal recycled material |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210407595.3ACN103011897B (en) | 2012-10-24 | 2012-10-24 | Preparation method of sapphire crystal recycled material |
| Publication Number | Publication Date |
|---|---|
| CN103011897Atrue CN103011897A (en) | 2013-04-03 |
| CN103011897B CN103011897B (en) | 2014-08-06 |
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210407595.3AActiveCN103011897B (en) | 2012-10-24 | 2012-10-24 | Preparation method of sapphire crystal recycled material |
| Country | Link |
|---|---|
| CN (1) | CN103011897B (en) |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103541009A (en)* | 2013-08-20 | 2014-01-29 | 曾锡强 | Recycling method of sapphire crystal residue |
| CN104131354A (en)* | 2013-05-02 | 2014-11-05 | 周黎 | Recycling method of residual crystal scrap after processing of sapphire crystal |
| CN104441279A (en)* | 2014-10-31 | 2015-03-25 | 镇江环太硅科技有限公司 | Cutting method for polycrystalline silicon ingot |
| CN104984794A (en)* | 2015-07-27 | 2015-10-21 | 鸿福晶体科技(安徽)有限公司 | Method for using waste seed crystal strip as grinding body for high purity alumina powder production |
| CN106000993A (en)* | 2016-05-12 | 2016-10-12 | 大工(青岛)新能源材料技术研究院有限公司 | Pollution-free silicon material crushing and cleaning method |
| CN112359418A (en)* | 2020-10-29 | 2021-02-12 | 福建晶安光电有限公司 | Crystal growth method |
| CN112725904A (en)* | 2020-12-09 | 2021-04-30 | 天通银厦新材料有限公司 | Method for recycling leftover material crystal shell material of sapphire crystal |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1395290A (en)* | 2002-06-28 | 2003-02-05 | 中国科学院上海微系统与信息技术研究所 | Gallium atom cleaning method of sapphire substrate for epitaxial growth |
| CN101468352A (en)* | 2007-12-27 | 2009-07-01 | 深圳市方大国科光电技术有限公司 | Method for cleaning sapphire substrate |
| CN102059747A (en)* | 2010-08-25 | 2011-05-18 | 重庆川仪自动化股份有限公司 | Method for forming sapphire square hole |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1395290A (en)* | 2002-06-28 | 2003-02-05 | 中国科学院上海微系统与信息技术研究所 | Gallium atom cleaning method of sapphire substrate for epitaxial growth |
| CN101468352A (en)* | 2007-12-27 | 2009-07-01 | 深圳市方大国科光电技术有限公司 | Method for cleaning sapphire substrate |
| CN102059747A (en)* | 2010-08-25 | 2011-05-18 | 重庆川仪自动化股份有限公司 | Method for forming sapphire square hole |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104131354A (en)* | 2013-05-02 | 2014-11-05 | 周黎 | Recycling method of residual crystal scrap after processing of sapphire crystal |
| CN103541009A (en)* | 2013-08-20 | 2014-01-29 | 曾锡强 | Recycling method of sapphire crystal residue |
| CN103541009B (en)* | 2013-08-20 | 2016-03-02 | 江西东海蓝玉光电科技有限公司 | A kind of reuse method of sapphire crystal residue material |
| CN104441279A (en)* | 2014-10-31 | 2015-03-25 | 镇江环太硅科技有限公司 | Cutting method for polycrystalline silicon ingot |
| CN104984794A (en)* | 2015-07-27 | 2015-10-21 | 鸿福晶体科技(安徽)有限公司 | Method for using waste seed crystal strip as grinding body for high purity alumina powder production |
| CN106000993A (en)* | 2016-05-12 | 2016-10-12 | 大工(青岛)新能源材料技术研究院有限公司 | Pollution-free silicon material crushing and cleaning method |
| CN112359418A (en)* | 2020-10-29 | 2021-02-12 | 福建晶安光电有限公司 | Crystal growth method |
| CN112725904A (en)* | 2020-12-09 | 2021-04-30 | 天通银厦新材料有限公司 | Method for recycling leftover material crystal shell material of sapphire crystal |
| Publication number | Publication date |
|---|---|
| CN103011897B (en) | 2014-08-06 |
| Publication | Publication Date | Title |
|---|---|---|
| CN103011897B (en) | Preparation method of sapphire crystal recycled material | |
| CN105948062B (en) | The preparation method of glass sand | |
| CN102092711A (en) | Method for preparing activated carbon from Chinese medicinal dregs | |
| CN103014591B (en) | Method for preparing infrared radiation amorphous coating | |
| CN102515175A (en) | Method for purifying quartz glass raw material | |
| CN104556047A (en) | Production process for preparing high-purity quartz powder from quartzite | |
| CN103966472A (en) | Method for removing iron in regenerated aluminum alloy | |
| CN105107192B (en) | A kind of go production method | |
| CN107364870B (en) | A kind of efficient impurity removal crushing process of fritting bottom seed crystal | |
| CN102583971A (en) | Hot-melting glass with bowlder effect and manufacturing method of hot-melting glass | |
| CN110498686A (en) | A kind of interlayer silicon carbide microwave heat structure crucible and preparation method thereof | |
| CN105200375A (en) | Preparation method of antibacterial stainless steel | |
| CN106077676A (en) | A kind of processing method of rare earth permanent magnet spent material | |
| CN105967213A (en) | Preparation method of calcium oxide | |
| CN104150535B (en) | A kind of method of synthesizing big L/D ratio flaky sodium niobate powder | |
| CN105903741A (en) | A clean regeneration process for waste glass | |
| CN102001655A (en) | Method for cleaning and recovering activating agent in production process of activated carbon | |
| CN106242282B (en) | A kind of ceramic glaze and preparation method thereof of absorbable electromagnetic radiation | |
| CN107721164A (en) | A kind of quartz glass of absorbable ultraviolet | |
| CN102384638A (en) | Drying box of lithium battery cathode material | |
| CN101698510A (en) | Ammonium vanadate drying method | |
| CN105837215A (en) | Preparation method of neodymium-yttrium-doped strontium fluoride laser transparent ceramic | |
| CN105032459A (en) | Microwave absorption foamed ceramic catalyst and preparation method thereof | |
| CN103583718A (en) | Aroma raising method for green tea | |
| CN101948762B (en) | Method for preparing active dry yeast by utilizing microwave vacuum drying |
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right | Effective date of registration:20240407 Address after:050035 No. 369, Zhujiang Avenue, high tech Zone, Shijiazhuang, Hebei Patentee after:TUNGHSU GROUP Co.,Ltd. Country or region after:China Address before:212218 Yangzhong Youfang Huantai Industrial Park, Zhenjiang City, Jiangsu Province Patentee before:JIANGSU JESHINE NEW MATERIAL Co.,Ltd. Country or region before:China | |
| PE01 | Entry into force of the registration of the contract for pledge of patent right | Denomination of invention:A method for preparing recycled sapphire crystal materials Granted publication date:20140806 Pledgee:Hengshui Bank Co.,Ltd. Pledgor:TUNGHSU GROUP Co.,Ltd. Registration number:Y2024980031994 | |
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right | Granted publication date:20140806 Pledgee:Hengshui Bank Co.,Ltd. Pledgor:TUNGHSU GROUP Co.,Ltd. Registration number:Y2024980031994 | |
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| TR01 | Transfer of patent right | Effective date of registration:20250522 Address after:Room 606, 6th Floor, Building D and E, Commercial Center, Renmin Road Central Street, Taocheng District, Hengshui City, Hebei Province 053099 Patentee after:Hengshui Hengyin Enterprise Management Co.,Ltd. Country or region after:China Address before:050035 No. 369, Zhujiang Avenue, high tech Zone, Shijiazhuang, Hebei Patentee before:TUNGHSU GROUP Co.,Ltd. Country or region before:China | |
| TR01 | Transfer of patent right |