CN102603007A - Preparation method of tungsten oxide nano powder and metal tungsten nano powder - Google Patents
Preparation method of tungsten oxide nano powder and metal tungsten nano powder Download PDFInfo
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 31
- 239000002184 metal Substances 0.000 title claims abstract description 31
- 239000011858 nanopowder Substances 0.000 title claims abstract description 31
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 31
- 239000010937 tungsten Substances 0.000 title claims abstract description 31
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000411 inducer Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001556 precipitation Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 8
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000006698 induction Effects 0.000 claims abstract description 3
- 239000003929 acidic solution Substances 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 10
- AAQNGTNRWPXMPB-UHFFFAOYSA-N dipotassium;dioxido(dioxo)tungsten Chemical compound [K+].[K+].[O-][W]([O-])(=O)=O AAQNGTNRWPXMPB-UHFFFAOYSA-N 0.000 claims description 3
- 239000012065 filter cake Substances 0.000 claims description 3
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 17
- 239000002244 precipitate Substances 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 7
- 229910001930 tungsten oxide Inorganic materials 0.000 description 7
- 239000000843 powder Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000000713 high-energy ball milling Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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Abstract
Description
一、技术领域 1. Technical field
本发明涉及制备氧化钨纳米粉体与金属钨纳米粉体的方法。The invention relates to a method for preparing tungsten oxide nanopowder and metal tungsten nanopowder.
二、背景技术 2. Background technology
金属钨具有高熔点、高硬度、耐磨损、良好的导电与导热性，在矿山、冶金、电子与机械等领域存在广泛的应用，同时也是制备硬质合金材料的重要原料。现代工业的快速发展对当今的硬质合金材料提出了更高要求，需要开发具有高硬度、高强度和高耐磨性的硬质合金材料。为改善传统硬质合金材料的综合机械性能，其有效途径之一是减少原料金属钨粉体的晶粒尺寸，获得高性能的超细粉体甚至纳米粉体，而生产金属钨超细粉体与纳米粉体又对原料氧化钨提出了更高的要求。Metal tungsten has a high melting point, high hardness, wear resistance, good electrical and thermal conductivity, and is widely used in the fields of mining, metallurgy, electronics and machinery, and is also an important raw material for the preparation of cemented carbide materials. The rapid development of modern industry has put forward higher requirements for today's cemented carbide materials, and it is necessary to develop cemented carbide materials with high hardness, high strength and high wear resistance. In order to improve the comprehensive mechanical properties of traditional hard alloy materials, one of the effective ways is to reduce the grain size of raw metal tungsten powder, obtain high-performance ultra-fine powder or even nano-powder, and produce metal tungsten ultra-fine powder And nano-powder puts forward higher requirements on the raw material tungsten oxide.
目前，国内外有关金属钨纳米粉体的制备方法较多，主要有高能球磨法、气体蒸发法、等离子体法、氧化钨还原法等。高能球磨方法成本低、工艺简单。但球磨过程中易混入杂质，生成的纳米粉体易于氧化；气体蒸发法是先将金属钨蒸发，再经液氮冷却后获得纳米粉体。因金属钨难以蒸发，需要消耗很高的能量；等离子体法属于一种高能物理方法，不仅能耗高，而且需要特殊的设备，生产成本高；氧化钨粉还原法是以联氨钨酸盐与仲钨酸铵等为原料，先合成出氧化钨，再经氢气还原获得金属钨纳米粉体，该法可以较好地控制纳米粉体的晶粒尺度，但金属钨的转化率较低，成本也相对较高。本发明以可溶性钨酸盐为主要原料，加入硫代乙酰胺充当诱导剂，通过酸化发生液相沉淀反应，可以方便地合成出氧化钨纳米粉体，经煅烧还原后可获得金属钨纳米粉体。硫代乙酰胺在酸性溶液中发生均匀水解，能均匀地释放出硫化氢气体，不仅可以维持溶液中的pH值，而且能够提供大量晶核，诱导氧化钨纳米粉体的生成。本发明合成工艺简单、反应快速、可以大批量生产，不仅可以获得氧化钨纳米粉体，经煅烧还原后还可获得金属钨纳米粉体。At present, there are many methods for preparing metal tungsten nanopowder at home and abroad, mainly including high-energy ball milling method, gas evaporation method, plasma method, tungsten oxide reduction method, etc. The high-energy ball milling method has low cost and simple process. However, impurities are easily mixed in the ball milling process, and the resulting nano-powder is easy to oxidize; the gas evaporation method first evaporates metal tungsten, and then obtains nano-powder after cooling with liquid nitrogen. Because metal tungsten is difficult to evaporate, it needs to consume a lot of energy; the plasma method is a high-energy physical method, which not only consumes high energy, but also requires special equipment and high production costs; the reduction method of tungsten oxide powder is based on hydrazine tungstate Using ammonium paratungstate as a raw material, first synthesize tungsten oxide, and then obtain metal tungsten nanopowder through hydrogen reduction. This method can better control the grain size of nanopowder, but the conversion rate of metal tungsten is relatively low, and the cost is relatively low. higher. The present invention uses soluble tungstate as the main raw material, adds thioacetamide as an inducer, and undergoes liquid-phase precipitation reaction through acidification to conveniently synthesize tungsten oxide nanopowder, which can be calcined and reduced to obtain metal tungsten nanopowder . Thioacetamide undergoes uniform hydrolysis in acidic solution, and can release hydrogen sulfide gas evenly, which can not only maintain the pH value in the solution, but also provide a large number of crystal nuclei to induce the formation of tungsten oxide nanopowders. The invention has the advantages of simple synthesis process, quick reaction and mass production, not only can obtain tungsten oxide nano powder, but also can obtain metal tungsten nano powder after calcining and reduction.
三、发明内容 3. Contents of the invention
本发明所提供的氧化钨纳米粉体与金属钨纳米粉体，尺寸小，分散均匀，是高性能的硬质合金原料。The tungsten oxide nanopowder and metal tungsten nanopowder provided by the invention are small in size and evenly dispersed, and are high-performance cemented carbide raw materials.
本发明所称的氧化钨纳米粉体与金属钨纳米粉体，是将钨酸盐与诱导剂溶解在适量的水中。在适宜的温度下，将酸性溶液加入到上述溶液中，随后出现沉淀反应。反应结束后，沉淀物经过滤、洗涤与干燥或在非还原性气氛下煅烧后，可获得氧化钨纳米粉体。将得到的氧化钨纳米粉体在还原性气氛中煅烧，便获得金属钨纳米粉体。The tungsten oxide nanopowder and metal tungsten nanopowder referred to in the present invention are dissolved tungstate and inducer in an appropriate amount of water. At an appropriate temperature, an acidic solution is added to the above solution, followed by a precipitation reaction. After the reaction, the precipitate is filtered, washed and dried or calcined in a non-reducing atmosphere to obtain tungsten oxide nanopowder. The obtained tungsten oxide nanopowder is calcined in a reducing atmosphere to obtain metal tungsten nanopowder.
氧化钨纳米粉体与金属钨纳米粉体，是利用硫代乙酰胺充当诱导剂，利用pH值小于或等于4的酸性溶液处理钨酸盐溶液，钨酸盐与酸发生快速的沉淀反应，先获得平均粒径约80nm的氧化钨纳米粉体，再经煅烧还原获得平均粒径约40nm的金属钨纳米粉体。Tungsten oxide nanopowder and metal tungsten nanopowder use thioacetamide as an inducer, and use an acidic solution with a pH value less than or equal to 4 to treat a tungstate solution. A rapid precipitation reaction occurs between tungstate and acid. A tungsten oxide nanopowder with an average particle diameter of about 80nm is obtained, and then calcined and reduced to obtain a metal tungsten nanopowder with an average particle diameter of about 40nm.
氧化钨纳米粉体与金属钨纳米粉体的合成方法，是在诱导剂硫代乙酰胺的诱导与调节下，以钨酸盐、酸性溶液与水为原料，按如下比例配备：The synthesis method of tungsten oxide nanopowder and metal tungsten nanopowder is under the induction and adjustment of the inducer thioacetamide, using tungstate, acidic solution and water as raw materials, and preparing according to the following ratio:
钨酸盐与诱导剂的质量比为1∶0.02-50；The mass ratio of tungstate to inducer is 1:0.02-50;
钨酸盐与酸性溶液的质量比为1∶0.1-2000；The mass ratio of tungstate to acidic solution is 1:0.1-2000;
钨酸盐与水的质量比为1∶1-10000。The mass ratio of tungstate to water is 1:1-10000.
然后将钨酸盐与诱导剂溶解在适量的水中，温度控制在0-100℃范围内。然后将酸性溶液加入到上述溶液中，随后出现沉淀反应。反应结束后进行过滤与洗涤，再将滤饼干燥或在非还原性气氛中煅烧，获得氧化钨纳米粉体。将得到的氧化钨纳米粉体在还原性气氛中经200-1200℃高温煅烧后，可获得金属钨纳米粉体。Then dissolve the tungstate and the inducer in an appropriate amount of water, and the temperature is controlled within the range of 0-100°C. An acidic solution is then added to the above solution, followed by a precipitation reaction. After the reaction is completed, filter and wash, and then dry the filter cake or calcinate it in a non-reducing atmosphere to obtain tungsten oxide nanopowder. After the obtained tungsten oxide nano powder is calcined at a high temperature of 200-1200° C. in a reducing atmosphere, metal tungsten nano powder can be obtained.
四、附图说明 4. Description of drawings
图1是利用本发明方法获得的氧化钨纳米粉体的透射电镜照片。图1中的氧化钨粉体平均粒径在80nm左右，分散均匀。图2是利用本发明方法获得的金属钨纳米粉体的透射电镜与扫描电镜照片，煅烧温度780℃。图2中的金属钨纳米粉体平均粒径在40nm左右。图3是本发明方法得到的氧化钨纳米粉体的X射线衍射图谱。图3符合氧化钨衍射特征，没有发现其它物相，表示产物纯度较高。图4是利用本发明方法获得的金属钨纳米粉体的X射线衍射图谱。图4符合金属钨的衍射特征，没有发现其它物相，表示产物纯度较高。Fig. 1 is a transmission electron micrograph of tungsten oxide nanopowder obtained by the method of the present invention. The average particle size of the tungsten oxide powder in Figure 1 is about 80nm, and the dispersion is uniform. Fig. 2 is a transmission electron microscope and a scanning electron microscope photograph of the metal tungsten nanopowder obtained by the method of the present invention, and the calcination temperature is 780°C. The average particle size of metal tungsten nanopowder in Fig. 2 is about 40nm. Fig. 3 is the X-ray diffraction spectrum of the tungsten oxide nanopowder obtained by the method of the present invention. Figure 3 conforms to the diffraction characteristics of tungsten oxide, and no other phases are found, indicating that the product has a high purity. Fig. 4 is an X-ray diffraction pattern of metal tungsten nanopowder obtained by the method of the present invention. Figure 4 conforms to the diffraction characteristics of metal tungsten, and no other phases are found, indicating that the product has a high purity.
五、具体实施方式 5. Specific implementation
实施例1：将1份钨酸钠与50份诱导剂溶解在4500份水中，加热上述溶液，然后在100℃下保温，同时用2000份pH＝4的酸性溶液处理，随后出现沉淀反应。反应结束后，沉淀物经过滤、洗涤与干燥，获得氧化钨纳米粉体。将得到的氧化钨纳米粉体在H2气氛中于1200℃下煅烧20分钟，获得金属钨纳米粉体。Example 1: Dissolve 1 part of sodium tungstate and 50 parts of inducer in 4500 parts of water, heat the above solution, and then keep it warm at 100°C, while treating it with 2000 parts of acidic solution with pH=4, followed by precipitation reaction. After the reaction, the precipitate is filtered, washed and dried to obtain tungsten oxide nanopowder. The obtained tungsten oxide nanopowder was calcined at 1200° C. for 20 minutes in H 2 atmosphere to obtain metallic tungsten nanopowder.
实施例2：将10份钨酸钾与1份诱导剂溶解在100份水中，加热上述溶液，然后在100℃下保温，同时用10份pH＝1的酸性溶液处理，随后出现沉淀反应。反应结束后，沉淀物经过滤、洗涤与干燥，获得氧化钨纳米粉体。将得到的氧化钨纳米粉体在CO气氛中于650℃下煅烧30分钟，获得金属钨纳米粉体。Example 2: Dissolve 10 parts of potassium tungstate and 1 part of inducer in 100 parts of water, heat the above solution, then keep it warm at 100°C, and treat it with 10 parts of acidic solution with pH=1, and then a precipitation reaction occurs. After the reaction, the precipitate is filtered, washed and dried to obtain tungsten oxide nanopowder. The obtained tungsten oxide nanopowder was calcined at 650° C. for 30 minutes in a CO atmosphere to obtain metal tungsten nanopowder.
实施例3：将10份钨酸铵与1份诱导剂溶解在100份水中，加热上述溶液，然后在50℃下保温，同时用10份pH＝1的酸性溶液处理，随后出现沉淀反应。反应结束后，将沉淀物过滤与洗涤，再将滤饼在N2下于500℃保温20分钟，获得氧化钨纳米粉体。将得到的氧化钨纳米粉体在H2气氛中于600℃下煅烧40分钟，获得金属钨纳米粉体。Example 3: Dissolve 10 parts of ammonium tungstate and 1 part of inducer in 100 parts of water, heat the above solution, then keep it warm at 50°C, and treat it with 10 parts of acidic solution with pH=1, followed by precipitation reaction. After the reaction, the precipitate was filtered and washed, and the filter cake was kept at 500° C. for 20 minutes under N 2 to obtain tungsten oxide nanopowder. The obtained tungsten oxide nanopowder was calcined at 600° C. for 40 minutes in H 2 atmosphere to obtain metal tungsten nanopowder.
实施例4：将1份钨酸钾与10份诱导剂溶解在100份水中，加热上述溶液，然后在80℃下保温，同时用100份pH＝2的酸性溶液处理，随后出现沉淀反应。反应结束后，沉淀物经过滤、洗涤与干燥，获得氧化钨纳米粉体。将得到的氧化钨纳米粉体在H2气氛中于600℃下煅烧60分钟，获得金属钨纳米粉体。Example 4: Dissolve 1 part of potassium tungstate and 10 parts of inducer in 100 parts of water, heat the above solution, then keep it warm at 80°C, and at the same time treat it with 100 parts of acidic solution with pH=2, followed by precipitation reaction. After the reaction, the precipitate is filtered, washed and dried to obtain tungsten oxide nanopowder. The obtained tungsten oxide nanopowder was calcined at 600° C. for 60 minutes in H 2 atmosphere to obtain metal tungsten nanopowder.
实施例5：将1份钨酸钠与2份诱导剂溶解在100份水中，加热上述溶液，然后在40℃下保温，同时用10份pH＝0.5的酸性溶液处理，随后出现沉淀反应。反应结束后，沉淀物经过滤、洗涤与干燥，获得氧化钨纳米粉体。将得到的氧化钨纳米粉体在H2气氛中于500℃下煅烧60分钟，获得金属钨纳米粉体。Example 5: Dissolve 1 part of sodium tungstate and 2 parts of inducer in 100 parts of water, heat the above solution, then keep it warm at 40°C, and treat it with 10 parts of acidic solution with pH=0.5, followed by precipitation reaction. After the reaction, the precipitate is filtered, washed and dried to obtain tungsten oxide nanopowder. The obtained tungsten oxide nanopowder was calcined at 500° C. for 60 minutes in H 2 atmosphere to obtain metal tungsten nanopowder.
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| WO2019061584A1 (en) * | 2017-09-30 | 2019-04-04 | 五邑大学 | Metal tungsten quantum dot preparation method |
| CN113264576A (en) * | 2021-05-17 | 2021-08-17 | 南昌航空大学 | All-solid-state WO3Tungsten mesh electrode material and preparation method and application thereof |
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| CN105126875B (en) * | 2015-07-16 | 2017-09-26 | 合肥学院 | A kind of tungsten disulfide/concave convex rod compound and preparation method thereof |
| CN105126875A (en) * | 2015-07-16 | 2015-12-09 | 合肥学院 | Tungsten disulfide/attapulgite composite and preparation method thereof |
| CN105692700A (en) * | 2016-01-12 | 2016-06-22 | 江苏科技大学 | Preparation method and application of tungsten trioxide nanoparticles capable of stably suspending in plating solution with high ion concentration |
| CN106006743A (en) * | 2016-05-31 | 2016-10-12 | 上海应用技术学院 | A kind of preparation method of orthorhombic black WO3 |
| WO2019061584A1 (en) * | 2017-09-30 | 2019-04-04 | 五邑大学 | Metal tungsten quantum dot preparation method |
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| CN113264576A (en) * | 2021-05-17 | 2021-08-17 | 南昌航空大学 | All-solid-state WO3Tungsten mesh electrode material and preparation method and application thereof |
| CN113955803A (en) * | 2021-11-02 | 2022-01-21 | 云南锡业集团（控股）有限责任公司研发中心 | Granularity-adjustable tungsten oxide powder and preparation method of tungsten powder |
| CN113955803B (en) * | 2021-11-02 | 2024-03-22 | 云南锡业集团（控股）有限责任公司研发中心 | Particle size-adjustable tungsten oxide powder and preparation method thereof |
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