CN102998320A - Far infrared material analysis and manufacturing method - Google Patents
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- CN102998320A CN102998320A CN2012103290312A CN201210329031A CN102998320A CN 102998320 A CN102998320 A CN 102998320A CN 2012103290312 A CN2012103290312 A CN 2012103290312A CN 201210329031 A CN201210329031 A CN 201210329031A CN 102998320 A CN102998320 A CN 102998320A
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Abstract
本发明公开一种远红外线材料的分析及制造方法，分析方法包括有：A.对一电气石加热至出现莫来石结晶相之工作温度；B.在该电气石上取得一观察剖面；C.在该观察剖面上区隔出莫来石结构区域与非莫来石结构区域；D.侦测该非莫来石结构区域的X光能谱，以确认该非莫来石结构区域所含成份内容；E.对该观察剖面进行结晶相分析，获得非莫来石结构区域的结晶相信息；F.根据所获得的非莫来石结构区域之成份与结晶相信息，作为调配远红外线材料的参考信息；其制造方法则在于选择相符成份，再将该成份加热至符合步骤E的结晶相，借以制作一远红外线材料。
The invention discloses an analysis and manufacturing method of a far-infrared material. The analysis method comprises: A. heating a tourmaline to a working temperature at which a mullite crystal phase appears; B. obtaining an observation section on the tourmaline; C. separating a mullite structure region and a non-mullite structure region on the observation section; D. detecting an X-ray energy spectrum of the non-mullite structure region to confirm the component content of the non-mullite structure region; E. performing a crystal phase analysis on the observation section to obtain crystal phase information of the non-mullite structure region; F. using the obtained component and crystal phase information of the non-mullite structure region as reference information for preparing a far-infrared material; and the manufacturing method comprises selecting a matching component and then heating the component to a crystal phase matching step E to manufacture a far-infrared material.
Description
技术领域 technical field
本发明是有关于一种远红外线材料分析及制造方法，特别是指针对电气石热性质与晶相进行分析，便可了解电气石中可以提高远红外线放射效率的矿物成份，借以能利用该等矿物成份制作一远红外线材料。 The present invention relates to a far-infrared material analysis and manufacturing method, especially to analyze the thermal properties and crystal phases of tourmaline, so as to understand the mineral components in tourmaline that can improve the radiation efficiency of far-infrared rays, so as to utilize these Mineral ingredients make a far infrared material.
背景技术 Background technique
目前一般所常见的远红外线组成物的制造方法，如中国台湾2008年11月16日所公开的发明第200844066号「远红外线组成物之制造方法及其制品」专利案，其揭露：以高温烧结远红外线材料，并研磨成微/奈米级的配方后，使该配方依附在一基材，制成一制品。由于该远红外线材料包含有配合该制品用途而决定比例的SiO2、AlO2、NaO2、K2O、MgO，因此，可以配合各种基材的不同，制成器皿、织物、薄膜、油漆、磁砖、燃料(汽油、柴油、瓦斯...等)、水的激化装置...等制品，使该特定制品利用前述配方的特性及微/奈米化活性(微/奈米效应，即比表面积增加)，大幅提升释放远红外线与负离子的效果。 Currently common far-infrared composition manufacturing methods, such as Invention No. 200844066 "Manufacturing method of far-infrared composition and its products" patent case published on November 16, 2008 in Taiwan, China, discloses: sintering at high temperature After the far-infrared material is ground into a micro/nano-scale formula, the formula is attached to a substrate to make a product. Since the far-infrared material contains SiO2, AlO2, NaO2, K2O, and MgO in proportions determined according to the use of the product, it can be made into containers, fabrics, films, paints, tiles, fuels, etc., in accordance with different substrates. (gasoline, diesel, gas... etc.), water intensification device... and other products, so that the specific product can use the characteristics of the aforementioned formula and micro/nano activity (micro/nano effect, that is, the increase in specific surface area) , greatly enhance the effect of releasing far infrared rays and negative ions.
该专利前案的远红外线组成物制造方法及其制品，可在常温下即能放射优质远红外线有效能量，但其并未揭露有能够利用电气石天然矿物制备出高放射率的远红外线材料，而且电气石种类繁多，目前亦无可以准确测试出可以放射出远红外线成分的方法，因此，在使用上仍有诸多的缺点。 The manufacturing method of the far-infrared ray composition and its products in the previous patent can emit high-quality far-infrared effective energy at room temperature, but it does not disclose that there is a far-infrared material with a high emissivity that can be prepared by using tourmaline natural minerals. Moreover, there are many kinds of tourmaline, and there is no method that can accurately test the components that can emit far-infrared rays at present. Therefore, there are still many shortcomings in use.
发明内容 Contents of the invention
爰此，有鉴于目前测试远红外线成分方法具有上述的缺点，故本发明提供一种远红外线材料分析及制造方法，包括有：A.对一电气石加热至出现莫来石结晶相之工作温度；B.在该电气石上取得一观察剖面；C.在该观察剖面上区隔出莫来石结构区域与非莫来石结构区域；D.侦测该非莫来石结构区域之X光能谱，以确认该非莫来石结构区域之所含成份内容；E.对该观察剖面进行结晶相分析，获得非莫来石结构区域之结晶相信息；F.根据步骤D与步骤E所获得之非莫来石结构区域之之成份与结晶相信息，作为调配远红外线材料之参考信息。 Therefore, in view of the above-mentioned shortcomings in the current method for testing far-infrared components, the present invention provides a method for analyzing and manufacturing far-infrared materials, which includes: A. heating a tourmaline to the working temperature at which the mullite crystal phase occurs ; B. Obtain an observation section on the tourmaline; C. Separate the mullite structure area and the non-mullite structure area on the observation section; D. Detect the X-ray energy of the non-mullite structure area Spectrum, to confirm the composition content of the non-mullite structure region; E. Conduct crystal phase analysis on the observed section to obtain the crystal phase information of the non-mullite structure region; F. Obtained according to steps D and E The composition and crystal phase information of the non-mullite structure region are used as reference information for the preparation of far-infrared materials.
上述步骤A的工作温度系介于1000℃至1600℃。 The working temperature of the above step A is between 1000°C and 1600°C.
上述步骤B是对该加热后电气石执行切削或/与研磨方式获得该观察剖面。 The above step B is to obtain the observation section by cutting or/and grinding the heated tourmaline.
上述步骤C是透过一电子显微镜，在该电气石的观察剖面上根据结晶形状区隔出莫来石结构区域与非莫来石结构区域。 The above step C is to separate the mullite structure area and the non-mullite structure area on the observation section of the tourmaline through an electron microscope according to the crystal shape.
上述步骤D是透过一能量散射光谱仪(EDS)来确认非莫来石结构区域的所含成份内容。 The above step D is to confirm the content of the components contained in the non-mullite structure region through an energy dispersive spectrometer (EDS).
上述步骤E是透过一X光绕射分析方法(XRD)来确认该非莫来石结构区域之结晶相。 The above step E is to confirm the crystal phase of the non-mullite structure region through an X-ray diffraction analysis method (XRD).
本发明亦可为一种远红外线材料制造方法，是根据上述远红外线材料分析方法的步骤D选择相符合的成份，再将该成份加热至符合步骤E的结晶相，以制作一远红外线材料。 The present invention can also be a kind of far-infrared material manufacturing method, is to select the corresponding composition according to step D of the above-mentioned far-infrared material analysis method, and then heats this composition to the crystalline phase that meets step E, to make a far-infrared material.
本发明所能达成的优点，是可针对不同的电气石，快速且简单的分析出非莫来石结构区域的基材中，具有高放射率远红外线的成份及结晶，借以可作为制造高放射率远红外线材料之用。 The advantage that the present invention can achieve is that it can quickly and simply analyze the components and crystals with high emissivity far-infrared rays in the substrate of the non-mullite structure region for different tourmalines, so that it can be used as a method for manufacturing high emissivity High rate far infrared material.
附图说明 Description of drawings
图1为本发明的操作步骤流程图， Fig. 1 is the flow chart of operation steps of the present invention,
图2为本发明电气石热性质分析示意图， Fig. 2 is a schematic diagram of tourmaline thermal property analysis of the present invention,
图3为本发明电气石经不同温度热处理的远红外线放射率， Fig. 3 is the far-infrared emissivity of tourmaline of the present invention through heat treatment at different temperatures,
图4为本发明电气石以不同温度热处理的XRD分析示意图， Fig. 4 is the XRD analysis schematic diagram of tourmaline of the present invention heat-treated at different temperatures,
图5为本发明电气石原观察剖面的微结构金相图， Fig. 5 is the microstructure metallographic diagram of tourmaline original observation section of the present invention,
图6为本发明电气石经850℃热处理后观察剖面的微结构金相图， Fig. 6 is the microstructural metallographic diagram of tourmaline of the present invention after observing section through 850 ℃ heat treatment,
图7为本发明电气石经950℃热处理后观察剖面的微结构金相图， Fig. 7 is the metallographic diagram of the microstructure of tourmaline of the present invention after 950 ℃ heat treatment of observed section,
图8为本发明电气石经1000℃热处理后观察剖面的微结构金相图， Fig. 8 is the metallographic diagram of the microstructure of tourmaline of the present invention after 1000 ℃ heat treatment of section observation,
图9为本发明电气石经1450℃热处理后在观察剖面的微结构所产生的局部丛状结晶金相图， Fig. 9 is the metallographic diagram of local cluster crystals produced by the tourmaline of the present invention after heat treatment at 1450°C in the microstructure of the observed section,
图10为本发明电气石经1450℃热处理后在观察剖面的微结构所产生的孔洞金相图， Fig. 10 is the metallographic diagram of the holes produced by the tourmaline of the present invention after heat treatment at 1450°C in the microstructure of the observed section,
图11为本发明电气石经1450℃热处理后在观察剖面的微结构所产生的完整针状莫来石金相图， Fig. 11 is a complete acicular mullite metallographic diagram produced by observing the microstructure of the section after the tourmaline of the present invention is heat-treated at 1450°C,
图12为本发明电气石经1450℃热处理后，对针状莫来石进行EDS的成份分析金相图， Fig. 12 is a metallographic diagram of EDS component analysis of acicular mullite after tourmaline of the present invention is heat-treated at 1450°C,
图13为本发明电气石中莫来石周边基材之EDS成份分析金相图， Fig. 13 is the EDS component analysis metallographic diagram of the surrounding base material of mullite in the tourmaline of the present invention,
图14为本发明电气石中基材的XRD矿物相分析示意图， Figure 14 is a schematic diagram of the XRD mineral phase analysis of the base material in tourmaline of the present invention,
表一为本发明电气石经EDS成份分析数据， Table one is tourmaline of the present invention through EDS component analysis data,
表二为本发明电气石经1450℃热处理后针状莫来石的EDS成份分析之数据， Table two is the data of the EDS component analysis of the acicular mullite after the tourmaline of the present invention is heat-treated at 1450°C,
表三为本发明电气石经1450°C热处理后的基材成份数据。 Table 3 is the base material composition data of the tourmaline of the present invention after heat treatment at 1450°C.
具体实施方式 Detailed ways
首先，请参阅图1所示，本发明为一种远红外线材料分析方法，包括有下列步骤： At first, referring to shown in Fig. 1, the present invention is a kind of far-infrared material analysis method, comprises the following steps:
A.对一电气石加热至出现莫来石结晶相的工作温度：其是对于一电气石进行加热的处理，使其工作温度系介于1000℃至1600℃之间，该电气石加热后进行热性质分析，如图2所示，在900℃至1000℃左右，有明显的重量损失及放热反应，而对于其进行远红外线放射率的分析〔如图3所示〕也显示出，远红外线放射率平均值从500℃开始有增强的现象，至950℃略降为0.955后，随着热处理温度的提高，远红外线放射率会继续提高；由于经过高温烧结的电气石其远红外线放射率有提高的现象，故可得知电气石在结构上的转变，是远红外线放射性能增强的因素；因此，特别针对电气石的热性质与晶相进行分析，便可了解电气石晶相的转变与放射性能提高的原因，再参考图4所示，电气石经各种温度进行热处理后，升温至850°C时，电气石的结构无太大的转变，而热处理温度提高至1000°C后，则开始产生莫来石矿物相，随着热处理温度的提高，莫来石的晶相强度有提高的现象，并对照图3所示的远红外线放射率，热处理温度越高者，远红外线的放射率越高，因此可证明与莫来石的产生有关； A. Heating a tourmaline to the working temperature at which the mullite crystal phase appears: it is a treatment for heating a tourmaline so that its working temperature is between 1000°C and 1600°C. After the tourmaline is heated, the The analysis of thermal properties, as shown in Figure 2, shows obvious weight loss and exothermic reaction at around 900°C to 1000°C, and the analysis of its far-infrared emissivity (as shown in Figure 3) also shows that far The average value of infrared emissivity increases from 500°C to 950°C and decreases slightly to 0.955. With the increase of heat treatment temperature, the far-infrared emissivity will continue to increase; because the far-infrared emissivity of tourmaline sintered at high temperature has increased Therefore, it can be known that the structural transformation of tourmaline is the factor that enhances the radioactivity of far-infrared rays; therefore, by analyzing the thermal properties and crystal phase of tourmaline, we can understand the transformation of tourmaline crystal phase and radioactivity. The reason for the improvement is shown in Figure 4. After the tourmaline is heat-treated at various temperatures, when the temperature is raised to 850°C, the structure of the tourmaline does not change much, and after the heat treatment temperature is increased to 1000°C, the The mullite mineral phase begins to be produced. As the heat treatment temperature increases, the crystal phase strength of the mullite increases. Compared with the far-infrared emissivity shown in Figure 3, the higher the heat treatment temperature, the far-infrared emissivity The higher, so it can be proved that it is related to the generation of mullite;
B.在该电气石上取得一观察剖面：对于该加热后的电气石，执行一切削或/与研磨方式，借以于该电气石上可以获得一个观察剖面； B. Obtain an observation section on the tourmaline: For the heated tourmaline, perform a cutting or/and grinding method, so as to obtain an observation section on the tourmaline;
C.在该观察剖面上区隔出莫来石结构区域与非莫来石结构区域：透过一电子显微镜（SEM），对于该电气石的观察剖面进行观察，电气石中存在着许多大小约为0.5 μm的结晶〔如图5所示〕，经由850℃热处理后晶粒会成长为大小约2μm的结晶〔如图6所示〕，电气石经950℃热处理后，其为结构开始产生裂纹，破断面整体上还可以辨别出矿物的结构，并且存在少许的晶粒〔如图7所示〕，经由1000℃热处理后，晶粒已完全消失，且有严重的纹路产生〔如图8所示〕，电气石经1450℃的热处理后，在表面会产生局部的丛状结晶〔如图9所示〕，在孔洞的部份则会明显观察到较为完整的针状莫来石〔如图10及第图11所示〕，在该电气石的观察剖面上根据结晶形状区隔出莫来石结构区域与非莫来石结构区域； C. Distinguish the mullite structure region and the non-mullite structure region on the observation section: through an electron microscope (SEM), observe the observation section of the tourmaline, there are many tourmalines with a size of about It is a crystal of 0.5 μm (as shown in Figure 5). After heat treatment at 850°C, the crystal grains will grow into crystals with a size of about 2 μm (as shown in Figure 6). After tourmaline is heat treated at 950°C, its structure begins to crack , the structure of the mineral can be identified on the broken surface as a whole, and there are a few crystal grains (as shown in Figure 7). After heat treatment at 1000°C, the grains have completely disappeared, and serious lines have occurred (as shown in Figure 8) Shown], after the tourmaline is heat-treated at 1450°C, local plexiform crystals will be produced on the surface (as shown in Figure 9), and relatively complete acicular mullite will be clearly observed in the part of the hole (as shown in Figure 9). 10 and shown in Figure 11], on the observation section of the tourmaline, the mullite structure region and the non-mullite structure region are separated according to the crystal shape;
D.侦测该非莫来石结构区域之X光能谱，以确认该非莫来石结构区域的所含成份内容：先对于该电气石的观察剖面，透过一能量散射光谱仪(EDS)来确认该电气石具有莫来石结构区域所含成份内容，如表1所示系为电气石的EDS成份分析，其中Al2O3的含量为35.92%，SiO2之含量为39.17%，如图9所示为电气石经1450°C热处理后，以EDS对电气石所产生的针状晶体进行成份分析，Al2O3的含量提高为43.25 %，SiO2含量降低为30.07 %〔如表2所示〕， D. Detect the X-ray energy spectrum of the non-mullite structure area to confirm the composition content of the non-mullite structure area: first, for the observation section of the tourmaline, through an energy dispersive spectrometer (EDS) To confirm that the tourmaline has the components contained in the mullite structure region, as shown in Table 1, it is the EDS composition analysis of tourmaline, wherein the content of Al2O3 is 35.92%, and the content of SiO2 is 39.17%, as shown in Figure 9 After the tourmaline is heat-treated at 1450°C, the composition of the needle-shaped crystals produced by the tourmaline is analyzed by EDS. The content of Al2O3 is increased to 43.25%, and the content of SiO2 is reduced to 30.07% [as shown in Table 2].
其成份中Al2O3与SiO2所产生的变化比例从1：1.09转变为1：0.7，而莫来石的典型组成中Al2O3与SiO2的比例为1：0.6，经热处理后，成份趋近于莫来石(Mullite)，因此可推断电气石经热处理后，其针状结晶应为莫来石，由于莫来石并非远红外线放射体，推测远红外线放射来源应是莫来石以外的基材，将电气石中已区隔出非莫来石结构之区域，透过该能量散射光谱仪(EDS)来确认非莫来石结构区域之基材所含成份内容〔如图10及图11所示〕，结果发现该基材成份中系已无Al2O3与SiO2之成份〔如表三所示〕。 The change ratio of Al2O3 and SiO2 in its composition changes from 1:1.09 to 1:0.7, while the ratio of Al2O3 to SiO2 in the typical composition of mullite is 1:0.6. After heat treatment, the composition is close to that of mullite (Mullite), so it can be inferred that after tourmaline is heat-treated, its needle-like crystals should be mullite. Since mullite is not a far-infrared emitter, it is speculated that the source of far-infrared radiation should be a substrate other than mullite. The non-mullite structure area has been separated in the stone, and the energy dispersive spectrometer (EDS) was used to confirm the content of the substrate in the non-mullite structure area (as shown in Figure 10 and Figure 11), and the results It is found that the base material has no Al2O3 and SiO2 components [as shown in Table 3]. the
表一 Table I
表二 Table II
表三 Table 3
E.对该观察剖面进行结晶相分析，获得非莫来石结构区域的结晶相信息：再透过一X光绕射分析方法(XRD)来确认该非莫来石结构区域的结晶相，经由XRD之绕射分析，并以图库分析比对出该基材的矿物相镁铁矿(Magnesioferrite)〔如图12及图13所示〕，在1450°C的XRD矿物相分析也显示莫来石相〔如图14所示〕，因此可推断电气石经热处理后，其针状结晶应为莫来石，由于对电气石进行热处理的温度越高，则莫来石的晶粒与结构越完整，相对的Mg、Fe、Na之氧化物之浓度也因为莫来石的析出而产生改变，由于莫来石并非远红外线的放射体，因此可以得知电气石中之Mg、Fe以及微量的Na为远红外线放射率提高之主因，借以取得非莫来石结构区域之结晶相相关的信息； E. Carry out crystal phase analysis on the observation section to obtain crystal phase information of the non-mullite structure region: then use an X-ray diffraction analysis method (XRD) to confirm the crystal phase of the non-mullite structure region, through Diffraction analysis of XRD, and the mineral phase Magnesioferrite (Magnesioferrite) of the substrate was compared with the library analysis (as shown in Figure 12 and Figure 13), and the XRD mineral phase analysis at 1450°C also showed mullite phase (as shown in Figure 14), so it can be inferred that after heat treatment of tourmaline, its needle-like crystals should be mullite, because the higher the temperature of heat treatment of tourmaline, the more complete the grain and structure of mullite , the relative concentration of Mg, Fe, and Na oxides also changes due to the precipitation of mullite. Since mullite is not a far-infrared emitter, it can be known that Mg, Fe, and a small amount of Na in tourmaline It is the main reason for the increase of far-infrared emissivity, so as to obtain information related to the crystal phase of the non-mullite structure region;
F.根据步骤D与步骤E所获得的非莫来石结构区域之之成份与结晶相信息，作为调配远红外线材料的参考信息：经由上述步骤D与步骤E确定，电气石中非莫来石结构区域之成份与结晶系为Mg、Fe以及微量的Na，故可针对加热后电气石进行分析的实验数据，以此数据利用Mg、Fe以及微量的Na，进行高放射率远红外线材料的成分调配。 F. According to the composition and crystal phase information of the non-mullite structure region obtained in step D and step E, it is used as reference information for the deployment of far-infrared materials: determined through the above steps D and E, non-mullite in tourmaline The composition and crystallization system of the structural region are Mg, Fe and a small amount of Na, so the experimental data can be analyzed for heated tourmaline, and the composition of the high emissivity far-infrared material can be determined using Mg, Fe and a small amount of Na. deployment.
本发明亦可为一种远红外线材料制造方法，其是根据上述远红外线材料分析方法，所获得具有高放射率远红外线材料的矿物成分数据，即包含有Mg、Fe以及微量的Na，然后选择与其相符合的矿物成份其中该相符合的成份，包含镁31-41%、铁49-59%及钠6-13%，再将该矿物成份加热至符合步骤E中具有高放射率远红外线材料之基材相同的结晶相，借以能制作完成一具有远红外线放射作用之材料。 The present invention also can be a kind of far-infrared ray material manufacturing method, and it is according to above-mentioned far-infrared ray material analysis method, the obtained mineral composition data with high emissivity far-infrared ray material, namely contains Mg, Fe and trace Na, then selects Wherein the corresponding mineral composition includes magnesium 31-41%, iron 49-59% and sodium 6-13%, and then the mineral composition is heated to meet the far-infrared material with high emissivity in step E The crystal phase is the same as that of the base material, so that a material with far-infrared radiation can be produced.
惟，以上所述仅为本发明其中之一最佳实施例，当不能以此限定本发明之申请专利保护范围，举凡依本发明之申请专利范围及说明书内容所作之简单的等效变化与替换，皆应仍属于本发明申请专利范围所涵盖保护之范围内。 However, the above description is only one of the best embodiments of the present invention, and should not limit the scope of patent protection of the present invention, for example, all simple equivalent changes and replacements made according to the patent scope of the present invention and the contents of the description , all should still belong to the scope of protection covered by the patent scope of the present invention application.
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| JPS58151380A (en) * | 1982-03-05 | 1983-09-08 | 旭硝子株式会社 | Far infrared ray radiator and manufacture |
| JPH1046426A (en) * | 1996-07-26 | 1998-02-17 | Brother Ind Ltd | Textile |
| CN1271758A (en) * | 2000-05-18 | 2000-11-01 | 上海维安热电材料有限公司 | Additive of efficient far infrared powder and its preparing process |
| CN101023793A (en) * | 2005-11-19 | 2007-08-29 | 丛繁滋 | Food, medicine preparation with far-infrared health-care function and assitant therapy functions and their preparing method |
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| JPS58151380A (en) * | 1982-03-05 | 1983-09-08 | 旭硝子株式会社 | Far infrared ray radiator and manufacture |
| JPH1046426A (en) * | 1996-07-26 | 1998-02-17 | Brother Ind Ltd | Textile |
| CN1271758A (en) * | 2000-05-18 | 2000-11-01 | 上海维安热电材料有限公司 | Additive of efficient far infrared powder and its preparing process |
| CN101023793A (en) * | 2005-11-19 | 2007-08-29 | 丛繁滋 | Food, medicine preparation with far-infrared health-care function and assitant therapy functions and their preparing method |
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| 陈俊良 等: "电气石之相变化与热分解产物之远红外线放射率研究", 《远东学报》, vol. 27, no. 2, 30 June 2010 (2010-06-30), pages 183 - 191 * |
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