CN117585990B - 一种黑色氧化铝基陶瓷基片及其制备方法 - Google Patents
一种黑色氧化铝基陶瓷基片及其制备方法 Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000000758 substrate Substances 0.000 title claims abstract description 38
- 239000000919 ceramic Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000003086 colorant Substances 0.000 claims abstract description 23
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 13
- 239000011230 binding agent Substances 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 44
- 238000010438 heat treatment Methods 0.000 claims description 23
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 11
- 229910006501 ZrSiO Inorganic materials 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 239000000395 magnesium oxide Substances 0.000 claims description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 8
- 235000010323 ascorbic acid Nutrition 0.000 claims description 7
- 229960005070 ascorbic acid Drugs 0.000 claims description 7
- 239000011668 ascorbic acid Substances 0.000 claims description 7
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 6
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 6
- 239000001639 calcium acetate Substances 0.000 claims description 6
- 235000011092 calcium acetate Nutrition 0.000 claims description 6
- 229960005147 calcium acetate Drugs 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 239000011258 core-shell material Substances 0.000 claims description 4
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- 229920004890 Triton X-100 Polymers 0.000 claims description 3
- 239000013504 Triton X-100 Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 230000007547 defect Effects 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000000593 microemulsion method Methods 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 4
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000049 pigment Substances 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 4
- 238000004040 coloring Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910017110 Fe—Cr—Co Inorganic materials 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
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- 238000011056 performance test Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
本发明涉及陶瓷材料领域，具体为一种黑色氧化铝基陶瓷基片及其制备方法，由氧化铝、着色剂、助剂和粘结剂制备而成；所述着色剂为核壳结构，其中核体为黑色TiO2‑x，x为含氧缺陷，0＜x＜2，壳体包括CaF2和ZrSiO4，本发明所制备的陶瓷基片具有优良的力学性能，市场应用前景广泛，且使用的着色剂不含Co、Cr等重金属元素，不会对环境和人体健康造成危害。
Description
技术领域
本发明涉及陶瓷材料领域，具体为一种黑色氧化铝基陶瓷基片及其制备方法。
背景技术
氧化铝陶瓷是目前应用最广泛的陶瓷封装基片材料，具有强度高、耐高温、耐热冲击性和电绝缘性及耐腐蚀性能力强等优良性能，且廉价易得。常见的氧化铝基片是白色，用作LED基板、高频电路基板等。但有些用途需要避免氧化铝基片反射光线，黑色氧化铝的产品因此生成。黑色氧化铝陶瓷基片多用于半导体集成电路及电子产品中，这主要是由于半导体集成电路以及某些电子产品具有明显的光敏性，要求作为封装材料的氧化铝陶瓷具有遮光性，为保证数码显示清晰也要求数码管衬板的氧化铝陶瓷呈黑色，黑色氧化铝基片在光电领域也有广泛的应用，由于黑色氧化铝基片具有良好的导热性能和光学性能，可以用作高功率激光器的散热基板。高功率激光器在工作过程中会产生大量的热量，如果不能及时散热，会导致激光器的温度升高，从而影响激光器的输出功率和寿命。而采用黑色氧化铝基片作为散热基板，可以有效地将激光器产生的热量迅速传导出去，保持激光器的正常工作温度，提高激光器的稳定性。
目前国内外制备黑色氧化铝一般采用一次合成法与二次合成法，一次合成法是将氧化铝、着色氧化物、助剂直接按一定的配比和工艺来制备黑色氧化铝，而二次合成法是先利用一些金属氧化物合成黑色色料，再把黑色色料、助溶剂、氧化铝按一定配比和工艺来制备黑色氧化铝。目前，常用的黑色色料为Fe-Co-Cr-Mn和Fe-Cr-Co系黑色色料，但是由于Co、Cr等重金属元素的加入，在生产过程中不可避免的会对人体健康造成危害。
发明内容
发明目的：针对上述技术问题，本发明提出了一种黑色氧化铝基陶瓷基片及其制备方法。
所采用的技术方案如下：
一种黑色氧化铝基陶瓷基片，由氧化铝、着色剂、助剂和粘结剂制备而成；
所述着色剂为核壳结构，其中核体为黑色TiO2-x，x为含氧缺陷，0＜x＜2，壳体包括CaF2和ZrSiO4。
进一步地，所述着色剂的壳体包括内层壳体和外层壳体，所述内层壳体为CaF2，所述外层壳体为ZrSiO4。
进一步地，所述着色剂的制备方法如下：
三氯化钛和抗坏血酸反应得到黑色TiO2-x，再采用溶液凝胶法和微乳液法在所述黑色TiO2-x的表面依次包覆CaF2和ZrSiO4即可。
进一步地，所述着色剂的制备方法如下：
将三氯化钛加入到抗坏血酸溶液中，用氢氧化钠溶液调整反应液pH至4-5，再将反应液转移至水热釜中，密封升温至180-200℃反应12-24h，冷却至室温后滤出沉淀，水洗、干燥后得到黑色TiO2-x，将三氟乙酸加入醋酸钙溶液中混匀得到溶胶，将黑色TiO2-x加入溶胶中搅拌均匀，加热蒸干、研磨，再升温至350-400℃热处理1-3h得到中间体，将曲拉通X-100、乙醇、环己烷、水混合均匀后再加入中间体，超声振荡后得到悬浮液，将正硅酸乙酯溶于乙醇/水混合液，得到溶液A，将氯氧化锆和氟化锂溶于水，得到溶液B，先将溶液A加入到悬浮液中，充分混匀后，再将溶液B加入，搅拌反应3-6h后，将固体滤出、洗涤得到前驱体，将其干燥后升温至900-950℃热处理0.5-2h即可。
进一步地，所述助剂包括氧化镁、氧化钇和氧化镧。
进一步地，所述氧化镁、氧化钇和氧化镧的重量比为1-5：1-5：1-5。
进一步地，所述粘结剂为聚乙烯醇粘结剂和/或石蜡基粘结剂。
进一步地，所述氧化铝、着色剂和助剂的重量比为90-100：1-5：0.1-1。
本发明还提供了一种黑色氧化铝基陶瓷基片的制备方法：
将氧化铝、着色剂、助剂混合球磨后再与粘结剂混匀，干燥、过筛、造粒，压制成坯后一段升温至600-650℃保温排胶1-2h，再二段升温至1350-1500℃烧结2-4h。
进一步地，一段升温的速度为10-20℃/min，二段升温的速度为1-5℃/min。
本发明的有益效果：
本发明提供了一种黑色氧化铝基陶瓷基片，目前已有报道TiO2纳米颗粒的氢热处理可以在表面附近产生无定形层，形成有缺陷的黑色TiO2-x纳米颗粒。这种黑色TiO2-x纳米颗粒的研究多集中于光催化领域，发明人采用水热法制备了黑色TiO2-x，并创造性的将其作为陶瓷着色剂制备黑色氧化铝基陶瓷，相比于Fe-Co-Cr-Mn和Fe-Cr-Co系黑色色料，其不含Co、Cr等重金属元素，不会对环境和人体健康造成危害，但是由于黑色TiO2-x易被氧化，影响着色效果，发明人黑色TiO2-x的表面依次包覆CaF2和ZrSiO4，形成双层包覆体系，避免TiO2-x被氧化，高熔点的ZrSiO4还可以避免CaF2被侵蚀，从而维持着色效果，核壳结构的着色剂能够以多种方式阻碍氧化铝基陶瓷中裂纹的扩展，如裂纹的钝化、偏转、钉扎及拔出等，使得氧化铝基陶瓷的抗弯强度和断裂韧性得以提高，本发明所制备的陶瓷基片具有优良的力学性能，市场应用前景广泛，且使用的着色剂不含Co、Cr等重金属元素，不会对环境和人体健康造成危害。
附图说明
图1为实施例1中所制备着色剂的照片。
图2为实施例1中所制备黑色氧化铝基陶瓷基片的照片。
具体实施方式
实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。本发明未提及的技术均参照现有技术，除非特别指出，以下实施例和对比例为平行试验，采用同样的处理步骤和参数。
实施例1：
一种黑色氧化铝基陶瓷基片，由重量比为95：2：0.6：25的氧化铝、着色剂、助剂和聚乙烯醇粘结剂制备而成；
其中，助剂由重量比为1：1：1的氧化镁、氧化钇和氧化镧组成；
着色剂为核壳结构，核体为黑色TiO2-x，x为含氧缺陷，0＜x＜2，壳体包括内层壳体和外层壳体，内层壳体为CaF2，外层壳体为ZrSiO4，着色剂的制备方法如下：
将70g抗坏血酸溶于5L去离子水中，得到抗坏血酸溶液，分多次将500g三氯化钛加入到抗坏血酸溶液中，用1M氢氧化钠溶液调整反应液pH至4，再将反应液转移至水热釜中，密封升温至180℃反应18h，冷却至室温后滤出沉淀，去离子水洗涤至中性后，80℃干燥24h后得到黑色TiO2-x，将15.8g醋酸钙溶于100ml去离子水中得到醋酸钙溶液，将22.8g三氟乙酸加入醋酸钙溶液中机械搅拌60min得到溶胶，取50g黑色TiO2-x加入溶胶中搅拌均匀，加热至80℃蒸干水分、研磨，再于氩气保护下升温至360℃热处理2h得到中间体，将80g曲拉通X-100、60g乙醇、400g环己烷、68g水混合均匀后再加入20g中间体，超声振荡30min后得到悬浮液，将20.8g正硅酸乙酯溶于100ml50％乙醇/水混合液，得到溶液A，将17.8g氯氧化锆和0.5g氟化锂溶于100ml去离子水中，得到溶液B，先将溶液A滴加入到悬浮液中，充分混匀后，再将溶液B滴加入，搅拌反应5h后，将固体滤出，用去离子水和乙醇反复洗涤后得到前驱体，将前驱体干燥后转移至马弗炉中于氩气保护下升温至950℃热处理1h即可。
上述黑色氧化铝基陶瓷基片的制备方法：
将氧化铝、着色剂、氧化镁、氧化钇和氧化镧混合球磨5h后干燥，与浓度为5wt％的聚乙烯醇粘结剂混匀，再经干燥、过筛、造粒后送入到冷等静压机内压制成型得到坯体，压力为150MPa，时间为10s，将坯体送入烧结炉中以15℃/min的速度一段升温至650℃保温排胶1.5h，再以5℃/min的速度二段升温至1450℃烧结2h，恢复室温后取出，肉眼观察到所制备的陶瓷基片为深黑色。
实施例2：
与实施例1基本相同，区别在于，助剂由重量比为3：2：1的氧化镁、氧化钇和氧化镧组成，恢复室温后取出，肉眼观察到所制备的陶瓷基片为深黑色。
实施例3：
与实施例1基本相同，区别在于，助剂由重量比为1：2：3的氧化镁、氧化钇和氧化镧组成，恢复室温后取出，肉眼观察到所制备的陶瓷基片为深黑色。
对比例1：
与实施例1基本相同，区别在于，直接加入黑色TiO2-x，不经过CaF2和ZrSiO4包覆处理，肉眼观察到所制备的陶瓷基片为灰白色。
对比例2：
与实施例1基本相同，区别在于，黑色TiO2-x只经过CaF2包覆处理，肉眼观察到所制备的陶瓷基片为深灰褐色。
对比例3：
与实施例1基本相同，区别在于，黑色TiO2-x只经过ZrSiO4包覆处理，肉眼观察到所制备的陶瓷基片为浅灰褐色。
性能测试：
将本发明实施例1-3及对比例1-3中的陶瓷基片制成试样，采用电子万能试验机测试试样的三点抗弯强度，测试间距为30mm，速率为0.5mm/min，单位MPa；
采用裂纹压痕技术在材料试验机上测试试样的断裂韧性，单位MPa·m1/2；测试结果如表1所示：
表1：
由上表1可知，本发明所制备的陶瓷基片具有优良的力学性能，市场应用前景广泛。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (6)
1.一种黑色氧化铝基陶瓷基片，其特征在于，由氧化铝、着色剂、助剂和粘结剂制备而成；
所述氧化铝、着色剂和助剂的重量比为90-100：1-5：0.1-1；
所述着色剂为核壳结构，其中核体为黑色TiO2-x，x为含氧缺陷，0＜x＜2，壳体包括CaF2和ZrSiO4；
所述着色剂的壳体包括内层壳体和外层壳体，所述内层壳体为CaF2，所述外层壳体为ZrSiO4；
所述助剂包括氧化镁、氧化钇和氧化镧；
所述氧化镁、氧化钇和氧化镧的重量比为1-5：1-5：1-5。
2.如权利要求1所述的黑色氧化铝基陶瓷基片，其特征在于，所述着色剂的制备方法如下：
三氯化钛和抗坏血酸反应得到黑色TiO2-x，再采用溶液凝胶法和微乳液法在所述黑色TiO2-x的表面依次包覆CaF2和ZrSiO4即可。
3.如权利要求2所述的黑色氧化铝基陶瓷基片，其特征在于，所述着色剂的制备方法如下：
将三氯化钛加入到抗坏血酸溶液中，用氢氧化钠溶液调整反应液pH至4-5，再将反应液转移至水热釜中，密封升温至180-200℃反应12-24h，冷却至室温后滤出沉淀，水洗、干燥后得到黑色TiO2-x，将三氟乙酸加入醋酸钙溶液中混匀得到溶胶，将黑色TiO2-x加入溶胶中搅拌均匀，加热蒸干、研磨，再升温至350-400℃热处理1-3h得到中间体，将曲拉通X-100、乙醇、环己烷、水混合均匀后再加入中间体，超声振荡后得到悬浮液，将正硅酸乙酯溶于乙醇/水混合液，得到溶液A，将氯氧化锆和氟化锂溶于水，得到溶液B，先将溶液A加入到悬浮液中，充分混匀后，再将溶液B加入，搅拌反应3-6h后，将固体滤出、洗涤得到前驱体，将其干燥后升温至900-950℃热处理0.5-2h即可。
4.如权利要求1所述的黑色氧化铝基陶瓷基片，其特征在于，所述粘结剂为聚乙烯醇粘结剂和/或石蜡基粘结剂。
5.一种如权利要求1-4中任一项所述的黑色氧化铝基陶瓷基片的制备方法，其特征在于，将氧化铝、着色剂、助剂混合球磨后再与粘结剂混匀，干燥、过筛、造粒，压制成坯后一段升温至600-650℃保温排胶1-2h，再二段升温至1350-1500℃烧结2-4h。
6.如权利要求5所述的黑色氧化铝基陶瓷基片的制备方法，其特征在于，一段升温的速度为10-20℃/min，二段升温的速度为1-5℃/min。
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