CN1190262C - Material for removing impurity in inert gas and its use method - Google Patents
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Abstract
一种去除隋性气体中杂质的材料及其使用方法，涉及一种去除惰性气体氙、氪中的氟碳化合物杂质的材料及其使用方法。其特征在于该合金的重量百分比组成为：含铝10%-25%，含铪1%-2%，镧系稀土0.4%-5%，镍1%-3%，余量为锆和不可避免的杂质。其使用过程是在700℃-960℃温度，将进行活化处理2-3小时；在400℃-960℃温度下进行吸附气体杂质的气体净化过程，控制气体流量为0.5m3/h-10m3/h，工作压力为0.3 MPa-1.5MPa。本发明的惰性气体净化材料，不吸收惰性气体，特别具有清除氟碳化合物(CF4、C2F4)等特殊性质。纯化后惰性气体纯度大于99.9999%，O2小于0.5ppm，氟碳化合物含量小于3ppm。A material for removing impurities in an inert gas and a method for using the same, relating to a material for removing impurities of fluorocarbons in the inert gases xenon and krypton and a method for using the same. It is characterized in that the weight percent composition of the alloy is: 10%-25% aluminum, 1%-2% hafnium, 0.4%-5% lanthanide rare earth, 1%-3% nickel, and the balance is zirconium and unavoidable of impurities. Its use process is at a temperature of 700°C-960°C, and activation treatment will be carried out for 2-3 hours; at a temperature of 400°C-960°C, the gas purification process of adsorbing gas impurities will be carried out, and the gas flow rate will be controlled at 0.5m 3 /h-10m3/ h, the working pressure is 0.3MPa-1.5MPa. The inert gas purification material of the present invention does not absorb inert gas, and has special properties such as removing fluorocarbons (CF 4 , C 2 F 4 ). After purification, the purity of inert gas is greater than 99.9999%, O2 is less than 0.5ppm, and the content of fluorocarbons is less than 3ppm.
Description
(一)技术领域(1) Technical field
一种去除惰性气体中杂质的材料及其使用方法，涉及一种去除用于半导体、高纯金属工业、化学成份分析及各种特殊电光源、激光器件、电光器件，特别是大功率照明灯中充有的惰性气体氙、氪中的氟碳化合物杂质的材料及其使用方法。A material for removing impurities in inert gas and its use method, relating to a method for removing impurities used in semiconductor, high-purity metal industry, chemical composition analysis and various special electric light sources, laser devices, electro-optic devices, especially high-power lighting lamps Material filled with fluorocarbon impurity in inert gas xenon, krypton and method of use thereof.
(二)背景技术(2) Background technology
高纯惰性气体是半导体、高纯金属工业、化学成份分析、各种特殊电光源、激光器件及多种高纯原料及工艺过程必须采用的载体和保护气氛及重要原料，在现代科技与工业发展占有非常重要的地位。目前用于高纯惰性气体生产的方法有多种，气体的纯化方法有空气分离法、吸收法和吸附法等。用这种方法可以有效地去除活性气体的O2、N2、CO、H2O等杂质，满足一定的工业用途。但对于气体中含有氟碳化合物去除效果常常不很理想，处理后的惰性气体中的氟碳化合物含量高于50ppm，难以满足对惰性气纯度要求高的工业用途，如特殊电光源等对惰性气体要求。由于惰性气体纯度的影响，在大功率照明灯内部呈现雾状，灯丝发黑，影响了产品质量。对特殊用途的惰性气体，纯度的高低是非常重要的指标。在目前已有的气体提纯技术中，对惰性气体中，特别是氪气、氙气中的CF4与C2F6去除方法还没有十分有效的方法。High-purity inert gas is the carrier, protective atmosphere and important raw material that must be used in semiconductor, high-purity metal industry, chemical composition analysis, various special electric light sources, laser devices and various high-purity raw materials and processes. occupies a very important position. At present, there are many methods for the production of high-purity inert gas, and the purification methods of gas include air separation method, absorption method and adsorption method. This method can effectively remove O 2 , N 2 , CO, H 2 O and other impurities in the active gas, which can meet certain industrial purposes. However, the removal effect of fluorocarbons in the gas is often not very ideal. The content of fluorocarbons in the treated inert gas is higher than 50ppm, which is difficult to meet the industrial applications with high requirements for the purity of inert gases, such as special electric light sources and other inert gases. Require. Due to the influence of the purity of the inert gas, the inside of the high-power lighting lamp is foggy, and the filament is black, which affects the product quality. For inert gases for special purposes, the purity is a very important indicator. In the existing gas purification technology, there is no very effective method for the removal of CF 4 and C 2 F 6 in inert gases, especially krypton and xenon.
(三)发明内容(3) Contents of the invention
本发明的目的是针对上述已有技术存在的不足，提供一种在可以有效清除氟碳化合物的去除惰性气体中杂质的材料及其使用方法。The object of the present invention is to address the shortcomings of the above-mentioned prior art and provide a material for removing impurities in inert gas that can effectively remove fluorocarbons and its application method.
本发明的目的是通过以下技术方案实现的。The purpose of the present invention is achieved through the following technical solutions.
一种去除惰性气体中杂质的材料，其特征在于该材料为一种锆合金，该合金的重量百分比组成为：含铝10％-25％，含铪1％-2％，镧系稀土0.4％-5％，镍1％-3％，余量为锆和不可避免的杂质，其材料为0.05mm-2.5mm颗粒。A material for removing impurities in an inert gas, characterized in that the material is a zirconium alloy, and the weight percentage of the alloy is: 10%-25% of aluminum, 1%-2% of hafnium, and 0.4% of lanthanide rare earth -5%, nickel 1%-3%, the balance is zirconium and unavoidable impurities, the material of which is 0.05mm-2.5mm particles.
本发明的一种去除惰性气体中杂质的材料也可以是多孔粉末烧结体。A material for removing impurities in an inert gas according to the present invention may also be a porous powder sintered body.
本发明的一种去除惰性气体中杂质的材料的锆合金中含有重量百分比为1％-4％的金属钛元素。The zirconium alloy of the material for removing impurities in the inert gas of the present invention contains 1%-4% by weight of metal titanium element.
一种去除惰性气体中杂质的材料的使用方法，其特征在于其使用过程为：A method for using a material for removing impurities in an inert gas, characterized in that the use process is:
a.将用于去除惰性气体中杂质的材料装入带有出入口的净化气体的不锈钢容器内，抽真空排气至真空度为10-3Pa后，充入惰性气体、升温700℃-960℃温度、保温2-3小时，将进行活化处理；a. Put the material used to remove impurities in the inert gas into a stainless steel container with a clean gas inlet and outlet, vacuumize and exhaust to a vacuum degree of 10-3Pa, fill in the inert gas, and raise the temperature to 700°C-960°C , Insulation for 2-3 hours, will be activated;
b.将欲净化的惰性气体通入装有除气材料的容器中，在400℃-960℃温度下进行吸附气体杂质的气体净化过程，控制气体流量为0.5m3/h-10m3/h，工作压力为0.3MPa-1.5MPa。b. Pass the inert gas to be purified into a container with degassing material, carry out the gas purification process of adsorbing gas impurities at a temperature of 400°C-960°C, and control the gas flow rate to 0.5m 3 /h-10m 3 /h , working pressure is 0.3MPa-1.5MPa.
本发明的惰性气体净化材料，不吸收惰性气体。这种材料具有可以有效地清除氟碳化合物(CF4、C2F4)等特殊性质。纯化后惰性气体纯度大于99.9999％，氟碳化合物含量小于3ppm。经过本发明的方法净化氪、氙气体时，氪、氙气体中的C2F和C2F4含量均从10ppm降至0.5ppm，且气体损失率在低于5％，效果极其显著。The inert gas purification material of the present invention does not absorb inert gas. This material has special properties such as being able to effectively remove fluorocarbons (CF 4 , C 2 F 4 ). After purification, the purity of the inert gas is greater than 99.9999%, and the content of fluorocarbons is less than 3ppm. When the krypton and xenon gases are purified by the method of the present invention, the content of C2F and C2F4 in the krypton and xenon gases is reduced from 10ppm to 0.5ppm, and the gas loss rate is lower than 5%. The effect is extremely remarkable.
(四)具体实施方式(4) Specific implementation methods
一种去除惰性气体中杂质的材料，该材料为一种锆铝合金，其重量百分比组成为：含铝10％-25％，含铪1％-2％，镧系稀土0.4％-5％，镍1％-3％，余量为锆和不可避免的杂质，其材料为0.05mm-2.5mm的颗粒。A material for removing impurities in an inert gas, the material is a zirconium-aluminum alloy, and its weight percentage composition is: 10%-25% of aluminum, 1%-2% of hafnium, 0.4%-5% of lanthanide rare earth, Nickel 1%-3%, the balance is zirconium and unavoidable impurities, its material is 0.05mm-2.5mm particles.
本发明的一种去除惰性气体中杂质的材料也可以是多孔粉末烧结体。A material for removing impurities in an inert gas according to the present invention may also be a porous powder sintered body.
本发明的一种去除惰性气体中杂质的材料的锆合金中还含有重量百分比为1％-4％的金属钛元素。The zirconium alloy of the material for removing impurities in the inert gas of the present invention also contains 1%-4% by weight of metallic titanium element.
一种去除惰性气体中杂质的材料的使用方法，首先将去除惰性气体中杂质的材料，装入带有出入口的净化气体的不锈钢容器内，抽真空排气至真空度为10-3Pa后，充入惰性气体、升温700℃-960℃温度、保温2-3小时，进行活化处理；将欲净化的惰性气体通入装有除气材料的容器中，在400℃-960℃温度下进行吸附气体杂质的气体净化，控制气体流量为0.5m/h，工作压力为0.3MPa-1.5MPa。通常锆基合金与氟碳化合物气体杂质在一定的压力和温度下有足够反应时间就会发生，将惰性气体中的氟碳化合物气体杂质吸除掉，发生吸气反应，生成稳定的锆碳化合物及锆氟化合物，这些化合物起初产生在锆基合金颗粒表面，随着吸气反应的进行不断向颗粒内部扩散。由于该化合物在吸气反应发生的温度下不分解，从而使氙氪等惰性气体中除去氟碳化合物的反应稳定而持续。A method for using a material for removing impurities in an inert gas. First, put the material for removing impurities in an inert gas into a stainless steel container with an inlet and outlet for purifying gas, and then vacuumize and exhaust the material to a vacuum degree of 10 -3 Pa. Fill in inert gas, raise the temperature at 700°C-960°C, keep it warm for 2-3 hours, and perform activation treatment; put the inert gas to be purified into a container with degassing material, and perform adsorption at a temperature of 400°C-960°C For gas purification of gas impurities, the control gas flow rate is 0.5m/h, and the working pressure is 0.3MPa-1.5MPa. Usually, zirconium-based alloys and fluorocarbon gas impurities will have sufficient reaction time under a certain pressure and temperature, and the fluorocarbon gas impurities in the inert gas will be absorbed and removed, and a getter reaction will occur to form a stable zirconium carbon compound. And zirconium-fluorine compounds, these compounds are initially produced on the surface of zirconium-based alloy particles, and continuously diffuse into the particles as the gettering reaction proceeds. Since the compound does not decompose at the temperature at which the gettering reaction occurs, the reaction of removing fluorocarbons in inert gases such as xenon and krypton is stable and continuous.
本发明的去除惰性气体中杂质的材料在锆基合金中加入了铝、铪、镧系稀土、钛等元素，这些元素在一定条件下也可以同惰性气体中的杂质反应，生成稳定的化合物，并且由于这些元素与锆形成的合金的除气性能更加显著，提高了锆与气体杂质的反应速度，去除氟碳化合物的气体杂质。The material for removing impurities in the inert gas of the present invention adds elements such as aluminum, hafnium, lanthanide rare earths, titanium and the like to the zirconium-based alloy. These elements can also react with the impurities in the inert gas under certain conditions to form stable compounds. And because the degassing performance of the alloy formed by these elements and zirconium is more significant, the reaction speed between zirconium and gas impurities is improved, and the gas impurities of fluorocarbons are removed.
下面结合实例对本发明作进一步的说明。Below in conjunction with example the present invention will be further described.
实施例1Example 1
惰性气体净化材料的成份为含铝11％，含铪2％，镧系稀土5％，镍2％，余量为锆和不可避免的杂质，在720℃下活化处理2.5小时，净化气体过程的工作温度为450℃，工作压力为0.5MPa，气体流量0.5m3/h，为净化后气体中的活性气体杂质含量35ppm，气体中C2F6、CF4杂质含量≤3ppm。The composition of the inert gas purification material is 11% aluminum, 2% hafnium, 5% lanthanide rare earth, 2% nickel, and the balance is zirconium and unavoidable impurities. It is activated at 720°C for 2.5 hours. The working temperature is 450°C, the working pressure is 0.5MPa, the gas flow rate is 0.5m 3 /h, the active gas impurity content in the purified gas is 35ppm, and the C 2 F 6 and CF 4 impurity content in the gas is ≤3ppm.
实施例2Example 2
惰性气体净化材料的成份为含铝15％，含铪1.5％，镧系稀土3％，镍1％，余量为锆和不可避免的杂质，在950℃下活化处理2小时，净化气体过程的工作温度为600℃，工作压力为1MPa，气体流量5m3/h，为净化后气体中的活性气体杂质含量45ppm，气体中C2F6、CF4杂质含量≤3ppm。The composition of the inert gas purification material is 15% aluminum, 1.5% hafnium, 3% lanthanide rare earth, 1% nickel, and the balance is zirconium and unavoidable impurities. It is activated at 950°C for 2 hours. The working temperature is 600°C, the working pressure is 1MPa, the gas flow rate is 5m 3 /h, the active gas impurity content in the purified gas is 45ppm, and the C 2 F 6 and CF 4 impurity content in the gas is ≤3ppm.
实施例3Example 3
惰性气体净化材料的成份为含铝12％，含铪2％，镧系稀土4％，21％，含钛4％，余量为锆和不可避免的杂质，在800℃下活化处理1.5小时，净化气体过程的工作温度为680℃，工作压力为1.5MPa，气体流量9m3/h，为净化后气体中的活性气体杂质含量47ppm，气体中C2F6、CF4杂质含量≤3ppm。The composition of the inert gas purification material is 12% aluminum, 2% hafnium, 4% and 21% lanthanide rare earths, 4% titanium, and the balance is zirconium and unavoidable impurities. It is activated at 800°C for 1.5 hours, The working temperature of the gas purification process is 680°C, the working pressure is 1.5MPa, the gas flow rate is 9m 3 /h, the active gas impurity content in the purified gas is 47ppm, and the C 2 F 6 and CF 4 impurity content in the gas is ≤3ppm.
实施例4Example 4
惰性气体净化材料的成份为含铝25％，含铪1％，镧系稀土0.5％，镍1％，余量为锆和不可避免的杂质，在700℃下活化处理3小时，净化气体过程的工作温度为720℃，工作压力为1.5MPa，气体流量7m3/h，为净化后气体中的活性气体杂质含量38ppm，气体中C2F6、CF4杂质含量≤3ppm。The composition of the inert gas purification material is 25% aluminum, 1% hafnium, 0.5% lanthanide rare earth, 1% nickel, and the balance is zirconium and unavoidable impurities. It is activated at 700°C for 3 hours, and the process of purifying the gas The working temperature is 720°C, the working pressure is 1.5MPa, the gas flow rate is 7m 3 /h, the active gas impurity content in the purified gas is 38ppm, and the C 2 F 6 and CF 4 impurity content in the gas is ≤3ppm.
实施例5Example 5
惰性气体净化材料的成份为含铝10％，含铪1％，镧系稀土4％，镍2％，钛含量1％，余量为锆和不可避免的杂质，在880℃下活化处理2.5小时，净化气体过程的工作温度为720℃，工作压力为1.5MPa，气体流量7m3/h，为净化后气体中的活性气体杂质含量36ppm，气体中C2F6、CF4杂质含量≤3ppm。The composition of the inert gas purification material is 10% aluminum, 1% hafnium, 4% lanthanide rare earth, 2% nickel, 1% titanium, and the rest is zirconium and unavoidable impurities. Activated at 880°C for 2.5 hours , the working temperature of the gas purification process is 720°C, the working pressure is 1.5MPa, the gas flow rate is 7m 3 /h, the active gas impurity content in the purified gas is 36ppm, and the C 2 F 6 and CF 4 impurity content in the gas is ≤3ppm.
实施例6Example 6
惰性气体净化材料的成份为含铝13％，含铪1％，镧系稀土3％，镍2％，钛含量1％，余量为锆和不可避免的杂质，在880℃下活化处理2.5小时，净化气体过程的工作温度为470℃，工作压力为1.5MPa，气体流量7m3/h，为净化后气体中的活性气体杂质含量42ppm，气体中C2F6、CF4杂质含量≤3ppm。The composition of the inert gas purification material is 13% aluminum, 1% hafnium, 3% lanthanide rare earth, 2% nickel, 1% titanium, and the rest is zirconium and unavoidable impurities. Activation treatment at 880°C for 2.5 hours , the working temperature of the gas purification process is 470°C, the working pressure is 1.5MPa, the gas flow rate is 7m 3 /h, the active gas impurity content in the purified gas is 42ppm, and the C 2 F 6 and CF 4 impurity content in the gas is ≤3ppm.
实施例7Example 7
惰性气体净化材料的成份为含铝16％，含铪1％，镧系稀土0.5％，镍2％，钛含量1％，余量为锆和不可避免的杂质，在880℃下活化处理2.5小时，净化气体过程的工作温度为700℃，工作压力为1.0MPa，气体流量6m3/h，为净化后气体中的活性气体杂质含量38ppm，气体中C2F6、CF4杂质含量≤3ppm。The composition of the inert gas purification material is 16% aluminum, 1% hafnium, 0.5% lanthanide rare earth, 2% nickel, 1% titanium, and the rest is zirconium and unavoidable impurities. Activation treatment at 880°C for 2.5 hours , the working temperature of the gas purification process is 700°C, the working pressure is 1.0MPa, the gas flow rate is 6m 3 /h, the active gas impurity content in the purified gas is 38ppm, and the C 2 F 6 and CF 4 impurity content in the gas is ≤3ppm.
实施例8Example 8
惰性气体净化材料的成份为含铝20％，含铪1％，镧系稀土0.4％，镍2％，钛含量1％，余量为锆和不可避免的杂质，在880℃下活化处理2.5小时，净化气体过程的工作温度为930℃，工作压力为0.9MPa，气体流量1.2m3/h，为净化后气体中的活性气体杂质含量38ppm，气体中C2F6、CF4杂质含量≤3ppm。The composition of the inert gas purification material is 20% aluminum, 1% hafnium, 0.4% lanthanide rare earth, 2% nickel, 1% titanium, and the rest is zirconium and unavoidable impurities. Activation treatment at 880°C for 2.5 hours , the working temperature of the gas purification process is 930°C, the working pressure is 0.9MPa, the gas flow rate is 1.2m 3 /h, the active gas impurity content in the purified gas is 38ppm, and the C 2 F 6 and CF 4 impurity content in the gas is ≤3ppm .
实施例9Example 9
惰性气体净化材料的成份为含铝10％，含铪1％，镧系稀土5％，镍3％，钛含量3％，余量为锆和不可避免的杂质，在880℃下活化处理2.5小时，净化气体过程的工作温度为520℃，工作压力为1.5MPa，气体流量0.6m3/h，为净化后气体中的活性气体杂质含量38ppm，气体中C2F6、CF4杂质含量≤3ppm。The composition of the inert gas purification material is 10% aluminum, 1% hafnium, 5% lanthanide rare earth, 3% nickel, 3% titanium, and the rest is zirconium and unavoidable impurities. Activation treatment at 880°C for 2.5 hours , the working temperature of the gas purification process is 520°C, the working pressure is 1.5MPa, the gas flow rate is 0.6m 3 /h, the active gas impurity content in the purified gas is 38ppm, and the C 2 F 6 and CF 4 impurity content in the gas is ≤3ppm .
实施例10Example 10
惰性气体净化材料的成份为含铝13％，含铪1.5％，镧系稀土4％，镍2％，钛含量2％，余量为锆和不可避免的杂质，在880℃下活化处理2.5小时，净化气体过程的工作温度为720℃，工作压力为1.3MPa，气体流量7m3/h，为净化后气体中的活性气体杂质含量48ppm；气体中C2F6、CF4杂质含量≤3ppm。The composition of the inert gas purification material is 13% aluminum, 1.5% hafnium, 4% lanthanide rare earth, 2% nickel, 2% titanium, and the rest is zirconium and unavoidable impurities. Activation treatment at 880°C for 2.5 hours , the working temperature of the gas purification process is 720°C, the working pressure is 1.3MPa, and the gas flow rate is 7m 3 /h, which means that the active gas impurity content in the purified gas is 48ppm; the C 2 F 6 and CF 4 impurity content in the gas is ≤3ppm.
实施例11Example 11
惰性气体净化材料的成份为含铝17％，含铪1％，镧系稀上2％，镍1％，钛含量1％，余量为锆和不可避免的杂质，在880℃下活化处理2.5小时，净化气体过程的工作温度为720℃，工作压力为1.5MPa，气体流量10m3/h，为净化后气体中的活性气体杂质含量48ppm，气体中C2F6、CF4杂质含量≤3ppm。The composition of the inert gas purification material is 17% aluminum, 1% hafnium, 2% lanthanide, 1% nickel, 1% titanium, and the rest is zirconium and unavoidable impurities. It is activated at 880°C for 2.5 Hours, the working temperature of the gas purification process is 720°C, the working pressure is 1.5MPa, the gas flow rate is 10m 3 /h, the content of active gas impurities in the purified gas is 48ppm, and the content of C 2 F 6 and CF 4 impurities in the gas is ≤3ppm .
实施例12Example 12
惰性气体净化材料的成份为含铝19％，含铪1％，镧系稀土5％，镍1％，钛含量4％，余量为锆和不可避免的杂质，在880℃下活化处理2.5小时，净化气体过程的工作温度为860℃，工作压力为1.5MPa，气体流量14m3/h，为净化后气体中的活性气体杂质含量41ppm，气体中C2F6、CF4杂质含量≤3ppm。The composition of the inert gas purification material is 19% aluminum, 1% hafnium, 5% lanthanide rare earth, 1% nickel, 4% titanium, and the rest is zirconium and unavoidable impurities. Activated at 880°C for 2.5 hours , the working temperature of the gas purification process is 860°C, the working pressure is 1.5MPa, the gas flow rate is 14m 3 /h, the active gas impurity content in the purified gas is 41ppm, and the C 2 F 6 and CF 4 impurity content in the gas is ≤3ppm.
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| CN1990380B (en) * | 2005-12-30 | 2010-10-13 | 天津环煜电子材料科技有限公司 | Technique for purifying and recovering argon gas by rare earth lanthanide series radical alloy degasser in single-crystal silicon preparation |
| JP5202836B2 (en) * | 2006-12-01 | 2013-06-05 | 日本エア・リキード株式会社 | Xenon recovery system and recovery device |
| CN102100999B (en) * | 2009-12-16 | 2013-05-15 | 贵阳铝镁设计研究院有限公司 | Method for purifying inert gases and purifying device |
| CN101880796B (en) * | 2010-07-15 | 2012-06-13 | 南京信息工程大学 | Zirconium-nickel alloy and preparation method thereof |
| CN104307461B (en) * | 2014-10-24 | 2016-06-29 | 武汉钢铁(集团)公司 | Krypton, xenon purification getter and preparation method thereof |
| CN106512702A (en) * | 2016-12-08 | 2017-03-22 | 天津工业大学 | Online purification method for inert gases based on titanium metallic chemical properties |
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