CN100424148C - 热致变色材料 - Google Patents

热致变色材料 Download PDF

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CN100424148C
CN100424148C CNB01823268XA CN01823268A CN100424148C CN 100424148 C CN100424148 C CN 100424148C CN B01823268X A CNB01823268X A CN B01823268XA CN 01823268 A CN01823268 A CN 01823268A CN 100424148 C CN100424148 C CN 100424148C
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metal
thermochromism
temperature
mixture
coating
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CN1671816A (zh
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A·V·比尔凯
A·M·埃弗莫夫
M·D·麦克海洛夫
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OOO CORNING
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OOO CORNING
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Abstract

揭示了一种热致变色材料，它包含热致变色组分和粘合剂，其中，所述热致变色组分是以元素周期表第I、II、III、IV、V、VI、VII、VIII族重金属氧化物为基础的结晶相，选自以下通式的化合物：(i)(Bi2O3)1-z(MxOy)z，其中，z＝0-0.5，M选自重金属、碱金属、碱土金属或者它们的混合物，(ii)(MxOy)m(Bi2O3)nNb(Ta)2O5，其中，m＝0-1，n＝1-2，M选自重金属、碱金属、碱土金属或者它们的混合物，(iii)(MxOy)m(Bi2O3)nMo(W)O3，其中，m＝0-1，n＝0-12，M选自碱金属、碱土金属、重金属或者它们的混合物，(iv)(MxOy)m(MexOy)nMo(W，Cr)O3，其中，m＝0-1，n＝0-1，M选自碱金属/碱土金属、重金属以及它们的混合物，Me是重金属，(v)(MxOy)m(MexOy)nNb(Ta)2O5，其中，m＝0-1，n＝0-1，M选自碱金属、碱土金属、重金属以及它们的混合物，Me选自Cu(II)、Mn(II)、Mn(III)、Co(II)、Ni(II)、Cr(III)，以热致变色组分和粘合剂的重量百分数计，其比例为2∶98-98∶2；并揭示了这些化合物(i)-(v)作为热致变色组分的应用。

Description

热致变色材料
本发明涉及热致变色材料，具体是热致变色涂层，其颜色改变可用作温度的指示。热致变色材料的应用领域是使用热致变色材料涂层在家用电器。使用热致变色材料可以简单而有效地提醒消费者接触一个物品特定部位的危险。
家用电器热致变色涂层的要求如下：
●涂层应能预示某个处于可能导致燃烧的100-400℃的范围内的表面的温度。例如，由于表面的热辐射或者可见的红色，可以感知在炊具盖子的表面上的高温度。
●在加热-冷却循环过程中，颜色改变应该是可逆的，不会有老化和受热过度(失色)的效应。
●涂层直至最高操作温度(对立柜式器炉头灶来说为700℃，对其它装置来说为400℃)应该稳定。
●涂层应符合卫生工艺要求和有关毒性方面的标准。
根据这些要求，本领域已知的以有机化合物和液晶为基础的热致变色材料就不能使用，这是因为它们在高温(700℃)下不稳定，因此，它们在本发明背景中不予考虑。
本领域中已知一种以如下物质为基础的热致变色材料：以镉和汞的硫化物和硒化物作为热致变色组分；以硅酸铅珐琅(美国专利No.5 772 328和No.5 499597)或者硼硅酸盐玻璃(美国专利No.4 983 810)作为粘合剂。本技术已知的热致变色材料可以制得在高达700℃的温度能稳定的涂层。但是，就目前的标准来说，以上述物质为基础的涂层不能用来施加到家用电器的表面，这是因为镉和汞的毒性等级很高。
在美国专利No.4 983 810中揭示的方案被认为和申请主张的热致变色材料最接近，按照这种方案，所述热致变色材料包含：
●作为热致变色组分的通式为CdS1-xSex或者通式Zn1-yMnyO的化合物，其中，x＝0-0.8，y＝0.05-0.15；
●作为粘合剂的玻璃或者玻璃陶瓷，具体是硼硅酸盐玻璃；
●作为非热致变色或者低热致变色化合物，其颜色接近热致变色组分的颜色的化合物，例如，Pb3(SbO4)2或ZrO2与镨的合金。在加热时，这种组分在热致变色组分中用作颜色转变的内标。
以上已经提到镉组合物有毒，就可用于家用电器的毒性而言，它也不符合卫生工艺标准的要求。至于其说明书中的化合物Zn1-yMnyO，它的稳定温度只能达到400℃，而且由于氧化作用，其颜色转变也不是完全可逆的。
本发明的目的在于形成一种热致变色材料，它没有毒性，且在室温到400℃的温度变化中，其颜色变化是可逆的，并且其颜色转变可以反映小于200℃的温度变化，而在加热到700℃下时是稳定的。
通过所揭示的热致变色材料可以达到这一目的，此热致变色材料包含以元素周期表第I、II、III、IV、V、VI、VII、VIII族重金属氧化物结晶为基础的热致变色组分，以及以碱金属或碱土金属的硅酸盐、硼酸盐和磷酸盐为基础的纯组分或者混合物作为粘合剂，热致变色组分∶粘合剂的重量比例为2-98∶98-2。
为了加强热致变色的特征，所述热致变色材料可以另外还包含一种热稳定的非热致变色组分或者低热致变色组分，其漫反射极大的区域和所述基本热致变色组分漫反射光谱随温度发生变化所在的光谱范围相同或者接近。
本发明独特的特征在于所述热致变色组分，它选自以下化合物：
(i)通式为(Bi2O3)1-z(MxOy)z的氧化铋基化合物，其中，z＝0-0.5，M选自重金属、碱金属、碱土金属或者它们的混合物。例如，M是Zr(IV)、Hf(IV)、Sn(II)、Sn(IV)、Nb(V)、Ta(V)、Mo(VI)、W(VI)、Cr(III)、Mn(II)、Fe(III)、Co(II)、Ni(II)、Pb(II)、Ca(II)、Sr(II)、Ba(II)、Li、Na、K、Rb、Cs。
(ii)通式为(MxOy)m(Bi2O3)nNb(Ta)2O5的铌酸盐和钽酸盐，其中，m＝0-1，n＝1-2，M选自重金属、碱金属、碱土金属或者它们的混合物。例如，M是Na、K、Rb、Cs、Mg、Ca、Sr、Ba、Pb(II)、Co(II)、Ni(II)、Cr(III)、Cu(II)、Cu(I)。
(iii)通式为(MxOy)m(Bi2O3)nMo(W)O3的钼酸盐和钨酸盐，其中，m＝0-1，n＝0-12，M选自碱金属、碱土金属、重金属和它们的混合物，例如，M是Na、K、Rb、Cs、Mg、Ca、Sr、Ba、Sn、Ti、Zr、Pb(II)、Mn(II)、Mn(III)、Co(II)、Ni(II)、Cr(III)、Cu(II)。
(iv)通式为(MxOy)m(MexOy)nMo(W，Cr)O3的铬酸盐、钼酸盐、钨酸盐，其中，m＝0-1，n＝0-1，M选自碱金属、碱土金属、重金属以及它们的混合物，Me是重金属。例如，M是Na、K、Pb、Cs、Mg、Ca、Sr、Ba、Sn、Ti、Zr、Pb(II)，Me是Cu(II)、Mn(II)、Mn(III)、Co(II)、Ni(II)、Cr(III)。
(v)通式为(MxOy)m(MexOy)nNb(Ta)2O5的铌酸盐和钽酸盐，其中，m＝0-1，n＝0-1，M选自碱金属、碱土金属、重金属以及它们的混合物，Me选自Cu(II)、Mn(II)、Mn(III)、Co(II)、Ni(II)、Cr(III)。例如，M是Na、K、Rb、Cs、Mg、Ca、Sr、Ba、Sn、Ti、Zr、Pb(II)。
对于热致变色化合物Bi2O3或选自(ii)和(iii)的化合物，稳定的非热致变色或者低热致变色颜料的例子是蓝钴CoAl2O4或CoWO4或Col-xZnxWO4或CoMoO4。另一例子是作为热致变色组分的(Bi2O3)x(CrO3)x和作为热稳定颜料的Cr2O3的混合物。热致变色化合物与热致变色颜料的比例为50∶1-1∶30。
通常，热致变色现象和固态中的相变(多型性转变)有关。这种类型固态热致变色化合物的典型代表是某些碘汞酸盐，钛酸盐(tallium)、汞、银的碘化物，它们在相变点时发生清晰且可逆的颜色变化。(J.H.Day.Thermochromism ofInorganic Compounds。Chem.Rev.，68(1968)，669；K.Sone，Y.Fukuda。InorganicThernochromism.Springer-Verlag，Berlin e.a.，1987)。这些化合物随温度变化产生高对比度的颜色变化，但是它们仅在低温下能稳定存在。对于大多数的热致变色化合物，如Ag2HgI4，其最大允许温度不超过200℃(D.Negoin，T.Rosu.Electric，thermal and thermochromic properties of MxHgI4-typecompound，Rev.Chem.，45(1994)，201)。它无法用在如厨房炉具的热致变色涂层中，立柜式器炉头灶的温度会达到700℃。
在本领域中已知一种耐热的热致变色氧化物，它以铝-铬取代结构为主的化合物为基础，例如红宝石和尖晶石(C.P.Polle.The optical Spectra and color ofChromium Containing solids.J.Phys.Chem.Dolids，25(1964)，1169)。
本领域已知的红宝石d-元素(Al2-xCrxO3)和尖晶石(MgAl2-xCrxO4)以及本发明所要求保护的化合物的组合物，其热致变色并不是决定于温度改变所引起的相变，而是配位场作用力的改变。由于铝原子被铬原子取代，所以随铬浓度的增加，颜色发生改变，由于铬原子的半径比铝原子的大，故上述取代伴随着晶格变形。因此，这种热致变色现象仅仅是对铬的。
若这些化合物中铬浓度不高，它们呈粉红色。当铬浓度高时，这些化合物的颜色为绿色。粉红色晶体具有热致变色现象：当加热时，其颜色逐渐从低温下的粉红色变为高温下的绿色。但是，这一变化在200-900℃的温度范围内很慢。在室温到400℃这一最需要向消费者警告的温度范围内，红宝石和尖晶石中的颜色变化不足以将它们用作涂层的热致变色组分。
在本文中所揭示的热致变色组分的特征为：在宽温度范围内其颜色变化是可逆的，且温度变化100℃是可以看见的；因此，以它们为基础的涂层在高达至700℃是热稳定的。
本文中，第一次不仅仅发现了上述特征，而且，第一次还发现这种固体化合物出现随温度变化的强对比度颜色变化，并且在高达700℃的空气中稳定存在。
通过如下标准方法制得上述化合物：压制起始氧化物的混合物，之后在700-1100℃热处理4-100小时，视组成而异。所得化合物的相组成通过在双衍射测量计DRON-2上所作的X-射线相分析来确定，化学组成通过X-射线光谱分析来控制。
测量在室温到400℃的范围内变化的温度考虑粉末漫反射光谱，测试所得热致变色化合物的热致变色特征。为进行测量，使用分光光度计SF-26，它具有含加热器的特殊单元安装在分光光度计中，代替用于粉末样品的标准托盘(holder)。漫射吸收带的偏移或者光谱形状的改变指示出热致变色效应。
根据漫射光谱的类型以及样品随温度变化而产生的行为，可以通过两种方法来表征涂层的热致变色性质：
1.颜色随温度变化的速度。通过色图(颜色三角图)上用坐标为(x，y)的点来表征涂层的颜色，这些座标由反射光谱计算(M.M.Gurevich，E.F.Itsko，M.M.Seredenko.Optic properties of vanish-paint coatings.“khimiya”，L.1984)。热致变色速度可以用这一点随温度沿所述色图移动的速度来表征，即值：
TX = o ‾ x 2 + y 2 ∂ T
一个普通的专家能区分多达1万种颜色，如果他能在这些颜中比较两种颜色的话。即是说，如果TX≈2×10-4，操作者可以看出在冷热表面间约100℃的温度差别。对于上述美国专利中提供的硫化镉而言，该值约为3×10-4。通过这一方法来评价热致变色特征的优点在于其绝对性质：用来比较不同涂层的基础是它们的颜色。但是，由于实行这个方法要求沿整个光谱对复杂函数进行积分，因此这个方法很费力。而且，操作者的眼睛感知在光谱不同范围内的颜色变化存在差异：在蓝色范围内看见较小的TX值，在红色中则较大。
2.在许多情况下，当加热后发生吸收带边缘的偏移，大多数情况是向光谱的长波区域偏移反射光谱也逐渐出现变化的许多情况，反射光谱的这种行为对半导体如用作热致变色组分的镉、锌和汞的硫化物来说是特有的(见上述美国专利)。在温度为从室温开始的温度范围内，吸收带边缘的位置(即漫反射边缘)随温度线性变化，若通过能量单位来表示：
E(T)＝E(To)-β(T-To)
其中，β是表征吸收带边缘随温度偏移的温度系数。β值越大，表明所述化合物的热致变色性质越强。例如，对硫化镉，该值为：
β＝7×10-4eV/K
当评价了所述化合物的热致变色性质之后，将其粉末和粘合剂混合物，所述粘合剂选自硅酸盐、磷酸盐、硼酸盐或者它们的混合物，热致变色组分和粘合剂的总比例为2∶98-98∶2，并加入水，将所得组合物施加到玻璃、金属、或玻璃-陶瓷表面上。为了提高涂层和玻璃-陶瓷、玻璃或者陶瓷的粘合力，上述材料基底可以用磨料粉末或者借助砂轮进行凹槽切削来进行粗糙化。将其上施加了涂层的样品板置于炉子中，并根据化合物的组成，加热至500-970℃，保持10分钟到1小时。之后，测试涂层漫反射光谱随温度的变化。
光谱测试的结果表明：本发明申请中所要求保护的金属氧化物以及以此为基础的涂层具有热致变色性质，它可逆，在室温到400℃的温度变化中具有强烈且对比鲜明的颜色变化，并且在高达700℃的温度仍然稳定，因此，100℃的温度变化可以清晰可见。
通过以下实施例将更好地说明本发明，但是它们不会限制权利的范围，而是仅仅用于说明的目的。
实施例1
这一实施例将详细说明制备热致变色涂层的方法及其特征。以1∶1∶1的摩尔比，总加入量为20g，将铋、铅、钽的氧化物粉末混合。将此混合物液压机以大用为1000kg/cm2的压力压制成片。将该片置于炉子中温度在5小时内逐渐从室温升至800℃。在这一温度保温100小时，炉子变冷后，将样品片取出研磨成粉末，混合，再次压制并再次在800℃下放置100小时。X-射线相分析表明得到均匀的结晶化合物PbO-Bi2O3-Ta2O5。当从20℃加热到400℃时，这一化合物出现热致变色，其颜色变化从淡黄色到橙色。这种化合物的粉末和以下组成的玻璃料粉末混合：78Ba(PO3)2·22Pb(PO3)2，质量比为90∶10，然后，将水加入所述混合物中，并将所得组合物施加到一玻璃-陶瓷板的表面上。将具有涂层的此玻璃-陶瓷板置于炉子中，温度逐渐升至500℃，在这一温度下保持1小时。所得的涂层为淡黄色。图1表示了其反射光谱，它表明随温度升高，吸收带边缘向光谱的长波区域逐渐偏移，即所得涂层具有热致变色性质。作为此涂层的热致变色特征，可以考虑吸收带边缘的位置随温度的关系，例如，在反射系数为0.5时。在图2中揭示了这种相关关系。很明显，本发明涂层的吸收带边缘的位置和温度呈线性关系，如同半导体化合物的情况一样。所述涂层的边缘偏移系数的温度系数为：
β＝(7.4±0.3)×10-4eV/K。
所述涂层的热致变色性质也可以通过颜色变化速度TX＝2.3×10-4表征。这些值和含有硫化镉的涂层所获得的热致变色值差不多。
实施例2
类似于实施例1，化合物的组成为PbO·Bi2O3·2Ta2O5。所得化合物和最终配方大致为Al2O3·3P2O5的磷铝酸盐粘合剂混合。这种粘合剂的制备和使用是遵照文献所推荐的(M.M.Sychev.non-organic glues，l.Khymia，1986)。在用于涂层中的此混合物中，粘合剂(重新计算为固体物质)和热致变色组分的质量比等于1∶9。所述混合物施加到按实施例1所述方法制备的玻璃-陶瓷表面上。加热至450℃来干燥所述涂层，并在这一温度下保持1小时。通过类似于实施例1所述的方法检测涂层的性质。根据测试，这一涂层吸收带边缘偏移的温度系数值为：
β＝(6.7±0.4)×10-4eV/K。
实施例3
以类似于实施例1和2的方式完成所有步骤，但是所述热致变色组分的组成为PbO·Bi2O3·4Ta2O5，且使用磷酸镁作为粘合剂，其大致组成为2MgO·P2O5，比例为70∶30。在450℃下加热涂层1小时。这一涂层吸收带边缘偏移的温度系数值为：
β＝(8.2±0.3)×10-4eV/K。
实施例4
这一实施例将说明制备以含氧化铋的化合物为基础，且具有最大热致变色值的热致变色涂层。使用上述实施例1和2中相同的合成条件，制得组成为7Bi2O3·Nb2O5的热致变色组分。如实施例2所述，施加所述涂层。在图3中给出了在室温到400℃的温度范围内的反射光谱，图4中给出了吸收带边缘位置和温度的关系。很明显，对于这一特定的涂层，热致变色值为：
β＝12.3×10-4eV/K。
它对应于加热时的颜色变化：从室温下的淡黄色变化至400℃时的深橙色。
Figure C0182326800091
表1归纳了涂层吸收带偏移的温度系数值，这些涂层以其组成中包含氧化铋的其它48种化合物为基础形成。它们都是热致变色的，并且其热致变色性质依赖于在加热时吸收带边缘向光谱长波区域的偏移。
实施例5
这一实施例将说明使用铬酸盐作为热致变色涂层的组分。将当量的铬酸钾溶液和氯化钡深倾倒在一起形成淡黄色铬酸钡残留物。过滤所得残留物，并和玻璃珐琅TIT24的硼硅酸盐混合，其比例为30∶70。
加入水之后，所得混合物沉积在一玻璃板的表面上。将所述玻璃板置于陶瓷炉中，其中，最高温度为970℃，在这一温度下保持30分钟。涂层的反射光谱在图5中，而吸收带边缘和温度的关系在图6中。所得涂层在室温下具有略带绿色的黄色。当温度从室温升至400℃时，涂层的颜色变为淡橙色。
以其它铬酸盐为基础的涂层的热致变色性质列于下表2中。
表2
包含作为热致变色组分铬酸盐的涂层的热致变色性质
  组成   β，×10<sup>-4</sup>eV/K   组成   β，×10<sup>-4</sup>eV/K
  2BaO·CrO<sub>3</sub>   5.8   CaCrO<sub>4</sub>   7.6
  2ZnO·CrO<sub>3</sub>   6.2   KAl(CrO<sub>4</sub>)<sub>2</sub>   6.4
  SrCrO<sub>4</sub>   6.7   2SrO·CrO<sub>3</sub>   6.1
  PbCrO<sub>4</sub>   5.8   2BaCrO<sub>4</sub>·BaSO<sub>4</sub>   5.8
  2CaO·CrO<sub>3</sub>   5.8   K<sub>2</sub>CrO<sub>4</sub>   4.1
实施例6
这一实施例将说明金属铌酸盐、钽酸盐、钼酸盐和钨酸盐作为热致变色组分的应用，除了铌酸锡和钽酸锡以外。将摩尔比为1∶1的20g氧化铅和氧化铌压制成，在800℃下退火100小时。退火之后，将所述片研磨，混合并再次在800℃下退火100小时。退火之后，将所述片研磨。将9.5g所得热致变色化合物粉末和0.4g硅酸钾和0.1g硼酸混合。所得混合物在水中搅拌，并沉积在一陶瓷板的表面上，将该板在450℃下退火。所述涂层为淡黄色，它在400℃下变成深黄色。温度系数值β＝4.2×10-4。以相同方式施加以锡化合物为基础的涂层，但是所有和热致变色组分制备以及涂层退火有关的操作均在真空中进行。
表3显示了涂层吸收带边缘偏移的温度系数值，所述涂层以氧化铌、氧化钽、氧化钼、氧化钨以及重金属氧化物为基础。所有这些涂层可以通过本实施例6中所述的方法制备。
表3
用作热致变色组分的重金属的铌酸盐、钽酸盐、钼酸盐和钨酸盐的热致变色性质
  组成   β，×10<sup>-4</sup>eV/K   组成   β，×10<sup>-4</sup>eV/K
  SnNb<sub>2</sub>O<sub>6</sub>   6.4   KnbO<sub>3</sub>   2.8
  PbO 2Ta<sub>2</sub>O<sub>5</sub>   2.7   2ZnO Nb<sub>2</sub>O<sub>5</sub>   5.8
  PbO Ta<sub>2</sub>O<sub>5</sub>   8.0   2PbO Nb<sub>2</sub>O<sub>5</sub>   4.4
  2PbO Ta<sub>2</sub>O<sub>5</sub>   6.9   SnTa<sub>2</sub>O<sub>6</sub>   7.8
  2Ga<sub>2</sub>O<sub>3</sub>·Ta<sub>2</sub>O<sub>5</sub>   4.1   BaNb<sub>2</sub>O<sub>6</sub>   3.2
  TiO<sub>2</sub>·2WO<sub>3</sub>   5.3   CuNb<sub>2</sub>O<sub>6</sub>   3.4
  ZrO<sub>2</sub>·2Nb<sub>2</sub>O<sub>5</sub>   2.1   AlNb<sub>2</sub>O<sub>4</sub>   3.0
  PbWO<sub>4</sub>   7.0   WO<sub>3</sub>   7.1
  PbO.8MgO.2WO<sub>4</sub>   4.6   BaMoO<sub>4</sub>   2.2
  ZnWO<sub>4</sub>   2.7   ZnMoO<sub>4</sub>   2.0
  Kga(WO<sub>4</sub>)<sub>2</sub>   4.8   CaWO<sub>4</sub>   3.9
按照本发明，用过渡金属离子如钴、铜、铬、镍、锰着色的铌酸盐、钽酸盐、钨酸盐和钼酸盐也可以用作涂层中的热致变色组分。加热这些化合物时，由于吸收带边缘偏移以及吸收带形状变化，它们的颜色改变。以下的实施例将说明制备热致变色涂层的工艺，在这些涂层中，使用非有机化合物作为热致变色组分，这些化合物的颜色取决于其中存在的过渡金属离子。
实施例7
将20g摩尔比为1∶1的碳酸钴和氧化钨的充分研磨混合物置于加热至800℃的炉子中。所述样品在这一温度保持30小时，之后将温度升至1000℃，在这一温度下再保持30小时。使用硅酸钾作为粘合剂，施涂涂层，热致变色颜料和粘合剂的比例为95∶5。图7中给出了所述涂层的反射光谱。从此光谱明显可知，在加热含有作为热致变色组分的钨酸钴的涂层时，颜色改变和反射光谱蓝光区域中吸收带边缘与透明带以及在光谱绿光区域中钴吸收带的加宽有关。涂层颜色从室温下的深蓝色变到400℃下的深黄色。以所测最小和最大温度颜色为基础计算所得的热致变色值TX＝2.8×10-4。钨酸钴的颜色对比度可以通过用其它二价金属如钙、镁、锌稀释钴来提高。镍、铜和锰的适当化合物也有热致变色性质，它们也可以用来制备本发明的涂层。表4给出了由涂层的反射光谱计算而得的热致变色值，这些涂层包含作为热致变色组分的一种上述化合物。在作为例子的图8中，给出了以钼酸镍为基础的涂层的反射光谱。
表4
钴、镍、锰和铜化合物的热致变色性质
  组成   在T＝20℃下的颜色   TX，*10<sup>-4</sup>
  CoNb<sub>2</sub>O<sub>6</sub> 蓝   1.8
  CoTa<sub>2</sub>O<sub>6</sub>   粉红   1.4
  CoMoO<sub>4</sub>   紫   1.2
  Co<sub>0.8</sub>Mg<sub>0.2</sub>WO<sub>4</sub> 蓝   2.0
  Co<sub>0.4</sub>Mg<sub>0.6</sub>WO<sub>4</sub> 蓝   1.8
  Co<sub>0.9</sub>Pb<sub>0.1</sub>WO<sub>4</sub>   深蓝   3.2
  Co<sub>0.6</sub>Zn<sub>0.4</sub>WO<sub>4</sub>   亮蓝   3.4
  Mn<sub>0.1</sub>Zn<sub>0.9</sub>MoO<sub>4</sub>   橙   1.3
  NiWO<sub>4</sub>   黄绿   1.1
  NiMoO<sub>4</sub>   绿   1.1
  NiTa<sub>2</sub>O<sub>6</sub>   黄绿   1.2
  CuMoO<sub>4</sub>   黄   1.4
  CuWO<sub>4</sub>   浅褐-黄   1.5
本发明中，如果热致变色化合物包含至少两种具有反射光谱一定比例的组分，可以获得更强烈的颜色变化。其原理如下：如上述实施例所述，让涂层在其组成中包含以吸收带边缘逐渐向光谱长波区域偏移的热致变色化合物。而且，涂层包含根本不具有热致变色性质的颜料，且其最大反射处于热致变色组分以及收带边缘主生偏移(图9，b)的相同光谱区域中。在这种情况下，混合物的反射光谱将上两种化合物反射光谱的重叠(图9，c)。在开始位置，颜料反射带在混合物反射光谱上是可以辩认的，这是由于在低温下它在热致变色组分透明区域中。当加热时热致变色组分的吸收带边缘向光谱的长波区域偏移，并在颜料反射区域中开始吸收。最后，在这一光谱区域中的反射强度降至背景水平。这种效应对应于从着色颜料的颜色色调向高温下热致变色组分颜色的颜色变化。自然，若所述着色颜料也具有热致变色性，例如本发明的锌和钴化合物，那么热致变色性质会更高。
以下一些实施例将说明了本发明化合物的实施方式。
实施例8
在700℃空气中将15g氧化铋预退火，然后和1g市售热稳定的蓝色颜料-钴蓝(CoAl2O3)混合，并加入0.3g硅酸钾作为粘合剂。剧烈搅拌所得混合物，加入水，沉积在金属表面上并干燥。图9中给出了所得混合材料的反射光谱。涂层颜色从室温下的蓝色向400℃下的橙色变化。以图10所给出的数据为基础计算热致变色速度为TX＝6.0×10-4。因此，混合热致变色组分-氧化铋和非热致变色颜料-钴蓝，将会使热致变色性质增强至纯氧化铋热致变色性质的两倍。
实施例9
将通过实施例1所述方法制备的10g热致变色化合物PbO·Bi2O3·Ta2O5和10g市售蓝绿玻璃C3C18(非热致变色组分)混合，并加入0.2g硅酸钠。剧烈搅拌所得混合物，并沉积在一陶瓷板表面上。将具有涂层的板干燥，并在700℃下保持30分钟。在加热时，涂层颜色从灰蓝色变为灰黄色。以反射光谱的温度依赖性为基础计算得到的热致变色速度为2.8，比起始化合物的热致变色性高25％。
实施例10
将通过实施例7所述方法制备的10g热致变色组分Co0.6Zn0.4WO4和实施例4中制备的10g另一种热致变色组分-7Bi2O3·O3混合，并加入0.4g粘合剂-四硼酸钠。用水加入到所述混合物中，并沉积在一陶瓷板表面上。干燥所述涂层并在550℃下加热1小时。图11中给出了所得涂层的反射光谱。所述混合物的热致变色值为7.9×10-4，是单独化合物热致变色性的两倍以上。

Claims (5)

1. 一种热致变色材料，它包含一种热致变色组分和一种粘合剂，其中，所述热致变色组分是以元素周期表第I、II、III、IV、V、VI、VII、VIII族重金属氧化物为基础的结晶相，选自以下通式的化合物：
(i)(Bi2O3)1-z(MxOy)z，其中，z＝0-0.5，M选自重金属、碱金属、碱土金属或者它们的混合物，
所述热致变色组分和粘合剂的重量百分数之比为2∶98-98∶2，并且所述热致变色材料还包含热稳定的非热致变色颜料或者热致变色颜料，其漫反射最大的区域和所述基本热致变色组分漫反射光谱随温度发生变化所在的光谱范围相同或者接近。
2. 权利要求1所述的材料，其特征在于，所述热致变色材料包含热稳定的非热致变色颜料。
3. 权利要求1所述的材料，其特征在于，所述热致变色组分与热稳定颜料的比例为50∶1至1∶30。
4. 权利要求1-3任一项所述的材料，其特征在于，所述粘合剂选自碱金属、或碱土金属的硅酸盐、硼酸盐、磷酸盐，以及它们的混合物。
5. 权利要求1所述的材料，其特征在于，式(Bi2O3)1-z(MxOy)z表示的化合物选自8Bi2O30.5Cr2O3、7Bi2O3WO3、15Bi2O3Li2O、CaO3.3Bi2O3、7Bi2O3Cr2O3、4Bi2O3Cr2O3、0.98Bi2O30.02Cr2O3、Bi2O3MoO3、15Bi2O3Na2O、3Bi2O3CrO3、8Bi2O3CrO3、0.94Bi2O30.06Cr2O3、Bi2O3WO3、7Bi2O3MoO3、SrOBi2O3、5CaO7Bi2O3、5Bi2O3 CrO3和3Bi2O3WO3。
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