CN106698367A - Method for preparing titanium nitride-based composite material - Google Patents
Method for preparing titanium nitride-based composite material Download PDFInfo
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- CN106698367A CN106698367A CN201510777297.7A CN201510777297A CN106698367A CN 106698367 A CN106698367 A CN 106698367A CN 201510777297 A CN201510777297 A CN 201510777297A CN 106698367 A CN106698367 A CN 106698367A
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- 239000002131 composite material Substances 0.000 title claims abstract description 61
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 36
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 22
- 239000011159 matrix material Substances 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000011065 in-situ storage Methods 0.000 claims abstract description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- -1 polytetrafluoroethylene Polymers 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 21
- 229910052719 titanium Inorganic materials 0.000 claims 21
- 239000010936 titanium Substances 0.000 claims 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 6
- 229910052757 nitrogen Inorganic materials 0.000 claims 3
- 241000790917 Dioxys <bee> Species 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 8
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 238000001308 synthesis method Methods 0.000 abstract description 3
- 239000000969 carrier Substances 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 21
- 238000006243 chemical reaction Methods 0.000 description 20
- 239000000243 solution Substances 0.000 description 13
- 239000000758 substrate Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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Abstract
本发明公开了一种制备氮化钛基复合材料的方法，属于无机非金属纳米材料制备技术领域。该制备方法采用气相水热的手段对氮化钛基体进行可控的氧化，在其表面原位生长二氧化钛，进而获得以氮化钛为基的复合材料。通过控制制备工艺，可以获得不同两相比例的复合材料，是一种简单、高效的复合合成方法，特别是该方法获得的复合材料界面接触良好，保证了两相间的载流子的有效传输，同时解决了传统复合方法需要高温煅烧的难题。The invention discloses a method for preparing a titanium nitride-based composite material, which belongs to the technical field of preparation of inorganic non-metallic nanometer materials. The preparation method adopts gas-phase hydrothermal means to carry out controllable oxidation on the titanium nitride matrix, grows titanium dioxide on the surface in situ, and then obtains the titanium nitride-based composite material. By controlling the preparation process, composite materials with different two-phase ratios can be obtained, which is a simple and efficient composite synthesis method. In particular, the interface contact of composite materials obtained by this method is good, which ensures the effective transport of carriers between the two phases. At the same time, it solves the problem that the traditional composite method requires high temperature calcination.
Description
技术领域technical field
本发明涉及无机非金属纳米材料制备技术领域，具体为一种制备氮化钛基复合材料的方法。The invention relates to the technical field of preparation of inorganic non-metallic nanometer materials, in particular to a method for preparing titanium nitride-based composite materials.
背景技术Background technique
水热法(溶剂热)是指在特制的反应容器中，在一定温度下加热水溶液(或其他溶剂)，创造一个高温、高压的反应环境，促使一些常温常压下难以进行的反应得以进行。而气相水热法是指利用水热(溶剂热)环境的高温高压特点进行材料改性的方法，在此过程中需改性材料(基体)不与反应容器中的溶液进行接触，而只是利用该高温高压环境，在一定工艺条件下使材料表面发生变化。The hydrothermal method (solvothermal) refers to heating an aqueous solution (or other solvent) at a certain temperature in a special reaction vessel to create a high-temperature, high-pressure reaction environment to promote some reactions that are difficult to carry out under normal temperature and pressure. The gas phase hydrothermal method refers to the method of modifying materials by using the high temperature and high pressure characteristics of the hydrothermal (solvothermal) environment. In this process, the modified material (substrate) does not contact the solution in the reaction vessel, but only uses The high temperature and high pressure environment changes the surface of the material under certain process conditions.
氮化钛是一种熔点高、硬度大、具有优良的化学稳定性以及耐腐蚀性的材料，同时其具有优良的导电性，在涂层、光电材料以及超导材料等领域有着众多的研究。但正是由于氮化钛本身优异的化学稳定性，必然导致在以其为基进行复合材料的制备过程中，传统的合成方法往往得不到理想的效果。所以可以结合气相水热法的特点，开发一种制备氮化钛基复合材料的方法，是制备以高化学稳定性材料为基的复合材料领域，特别是低能耗材料制备领域的一个十分重要的研究方向。Titanium nitride is a material with high melting point, high hardness, excellent chemical stability and corrosion resistance. At the same time, it has excellent electrical conductivity. There are many researches in the fields of coatings, optoelectronic materials and superconducting materials. However, it is precisely because of the excellent chemical stability of titanium nitride itself that the traditional synthesis methods often fail to obtain ideal results in the preparation of composite materials based on titanium nitride. Therefore, it is possible to develop a method for preparing titanium nitride-based composite materials in combination with the characteristics of the gas-phase hydrothermal method. research direction.
发明内容Contents of the invention
本发明的目的在于提供一种制备氮化钛基复合材料的方法，利用气相水热高温高压的反应特点，通过控制制备工艺，对氮化钛基体进行可控的氧化，在其表面原位生长二氧化钛，进而可在较低的温度下实现具有不同两相比例的氮化钛基复合材料的合成。The purpose of the present invention is to provide a method for preparing titanium nitride-based composite materials. Using the reaction characteristics of gas phase hydrothermal high temperature and high pressure, by controlling the preparation process, the titanium nitride matrix can be controlled to oxidize and grow in situ on its surface. Titanium dioxide, in turn, can realize the synthesis of titanium nitride-based composite materials with different two-phase ratios at a lower temperature.
本发明的技术方案是：Technical scheme of the present invention is:
一种制备氮化钛基复合材料的方法，该方法采用气相水热方法对氮化钛基体进行氧化，在其表面原位生长二氧化钛，从而获得由氮化钛和二氧化钛两相组成的氮化钛基复合材料；该方法具体包括如下步骤：A method for preparing a titanium nitride-based composite material, the method adopts a gas-phase hydrothermal method to oxidize a titanium nitride matrix, and grows titanium dioxide on its surface in situ, thereby obtaining titanium nitride composed of two phases of titanium nitride and titanium dioxide matrix composite material; the method specifically includes the following steps:
(1)将氮化钛基体均匀置放于聚四氟乙烯载架上；(1) Place the titanium nitride substrate evenly on the polytetrafluoroethylene carrier;
(2)将载有氮化钛基体的载架放置于带有聚四氟乙烯内衬的反应釜中，反应釜内装有HNO3或HF溶液，密封后将反应釜置于烘箱，在150-180℃条件下反应1-12h；(2) Place the carrier carrying the titanium nitride substrate in a reaction kettle with a polytetrafluoroethylene liner. The reaction kettle is equipped with HNO3 or HF solution. After sealing, the reaction kettle is placed in an oven and heated at 150- React at 180°C for 1-12h;
(3)取出反应釜空冷至室温，将所得沉淀经离心和去离子水冲洗后，在60℃条件下干燥10-24h，即获得所述氮化钛基复合材料。(3) Take out the reaction kettle and air cool to room temperature, centrifuge and rinse the obtained precipitate with deionized water, and dry at 60°C for 10-24h to obtain the titanium nitride-based composite material.
上述步骤(1)中，所述氮化钛基体为薄膜状或粉末状的氮化钛材料。In the above step (1), the titanium nitride substrate is a thin film or powder titanium nitride material.
上述步骤(2)中，所述HNO3或HF溶液的浓度为0.01-1.0mol/L。In the above step (2), the concentration of the HNO3 or HF solution is 0.01-1.0mol/L.
上述步骤(2)中，置于反应釜内载架上的氮化钛基体位于HNO3或HF溶液液面的上方。In the above step (2), the titanium nitride substrate placed on the carrier in the reaction kettle is located above the liquid level of the HNO 3 or HF solution.
采用上述方法制备氮化钛基复合材料过程中，通过控制HNO3或HF溶液的浓度以及反应时间来调控所得氮化钛基复合材料中氮化钛和二氧化钛的两相比例，HNO3或HF溶液的浓度越高，所得复合材料中二氧化钛所占比例越大，反应时间越长，所得复合材料中二氧化钛所占比例越大。In the process of preparing titanium nitride-based composite materials by the above method, the two-phase ratio of titanium nitride and titanium dioxide in the obtained titanium nitride -based composite materials is regulated by controlling the concentration of HNO or HF solution and the reaction time, HNO or HF solution The higher the concentration, the greater the proportion of titanium dioxide in the obtained composite material, and the longer the reaction time, the greater the proportion of titanium dioxide in the obtained composite material.
经本发明上述方法制备获得的氮化钛基复合材料中，氮化钛和二氧化钛的两相比例范围为0-100％。In the titanium nitride-based composite material prepared by the above-mentioned method of the present invention, the two-phase ratio of titanium nitride and titanium dioxide is in the range of 0-100%.
本发明的设计原理如下：Design principle of the present invention is as follows:
本发明利用气相水热法在较低的能耗下能创造出一种高温高压的环境的特点，通过气相的氧化，使具有高化学稳定性的氮化钛材料表面发生氧化，原位生成二氧化钛，从而获得一种两相接触良好、比例可调的氮化钛基复合材料。通过该工艺合成的复合材料，由于具有良好的界面特性，有利于氮化钛与二氧化钛之间的载流子传输。The present invention utilizes gas-phase hydrothermal method to create a high-temperature and high-pressure environment with relatively low energy consumption. Through gas-phase oxidation, the surface of titanium nitride material with high chemical stability is oxidized, and titanium dioxide is generated in situ. , so as to obtain a titanium nitride-based composite material with good two-phase contact and adjustable ratio. The composite material synthesized by this process is beneficial to the carrier transport between titanium nitride and titanium dioxide due to its good interface properties.
本发明的优点在于：The advantages of the present invention are:
1.本发明通过简单的气相水热氧化法制备氮化钛基复合材料，该复合过程操作简单，易于控制，易于工业化生产。1. The present invention prepares the titanium nitride-based composite material through a simple vapor phase hydrothermal oxidation method, and the composite process is simple to operate, easy to control, and easy to industrialized production.
2.本发明的复合方法能可控的原位生长二氧化钛，从而调节复合材料中两相的比例，同时具有良好的界面特性，有利于两相间的载流子传输。2. The composite method of the present invention can controllably grow titanium dioxide in situ, thereby adjusting the ratio of the two phases in the composite material, and has good interface properties, which is beneficial to the carrier transport between the two phases.
3.本发明的方法相比传统的复合方法，具有能耗低的优点。3. Compared with the traditional composite method, the method of the present invention has the advantage of low energy consumption.
附图说明：Description of drawings:
图1为本发明制备氮化钛基复合材料所用装置结构示意图。Fig. 1 is a schematic diagram of the structure of the device used in the preparation of titanium nitride-based composite materials according to the present invention.
图2为本发明实施例3中样品3的XRD图。Fig. 2 is an XRD pattern of sample 3 in Example 3 of the present invention.
图3为本发明实施例3中样品3的TEM图片。Fig. 3 is a TEM picture of sample 3 in Example 3 of the present invention.
具体实施方式：detailed description:
以下结合附图及实施例详述本发明。The present invention will be described in detail below in conjunction with the accompanying drawings and embodiments.
本发明采用气相水热的手段对氮化钛基体进行可控的氧化，在其表面原位生长二氧化钛，进而获得以氮化钛为基的复合材料。以下实施例在制备氮化钛基复合材料的过程中，所用装置如图1所示，该装置包括带有聚四氟乙烯内衬的反应釜和载架，载架为圆柱状结构。使用时，将氮化钛基体均匀置于载架的上表面上，然后将载架放入反应釜内，釜的底部装有反应用溶液。The invention adopts gas-phase hydrothermal means to carry out controllable oxidation on the titanium nitride substrate, grows titanium dioxide on the surface in situ, and then obtains the composite material based on the titanium nitride. In the following examples, in the process of preparing titanium nitride-based composite materials, the device used is shown in Figure 1. The device includes a reaction kettle with a polytetrafluoroethylene liner and a carrier, and the carrier is a cylindrical structure. When in use, the titanium nitride substrate is evenly placed on the upper surface of the carrier, and then the carrier is put into a reaction kettle, and the bottom of the kettle is equipped with a solution for reaction.
实施例1Example 1
1)按5mg/cm2的比例，将氮化钛粉末均匀置放于聚四氟乙烯载架上；1) According to the ratio of 5mg/ cm2 , the titanium nitride powder is evenly placed on the polytetrafluoroethylene carrier;
2)将载架放置入装有15mL浓度为0.1mol/L的HNO3溶液的反应釜中，密封后置于烘箱，在180℃条件下反应1h；2) Place the carrier into a reaction kettle filled with 15mL of HNO3 solution with a concentration of 0.1mol/L, seal it and place it in an oven, and react at 180°C for 1h;
3)取出反应釜空冷到室温，将所得沉淀反复离心和去离子水冲洗，在60℃温度下干燥12h，获得氮化钛基复合材料样品1。3) Take out the reaction kettle and air cool it to room temperature, centrifuge the obtained precipitate repeatedly and wash it with deionized water, and dry it at 60° C. for 12 hours to obtain a titanium nitride-based composite material sample 1 .
实施例2Example 2
1)按5mg/cm2的比例，将氮化钛粉末均匀置放于聚四氟乙烯载架上；1) According to the ratio of 5mg/ cm2 , the titanium nitride powder is evenly placed on the polytetrafluoroethylene carrier;
2)将载架放置入装有15mL浓度为0.1mol/L的HNO3溶液的反应釜中，密封后置于烘箱，在180℃条件下，反应2h；2) Place the carrier into a reaction kettle filled with 15mL of HNO 3 solution with a concentration of 0.1mol/L, seal it and place it in an oven, and react for 2 hours at 180°C;
3)取出反应釜空冷到室温，将所得沉淀反复离心和去离子水冲洗，在60℃温度下干燥12h，获得氮化钛基复合材料样品2。3) Take out the reactor and air cool it to room temperature, centrifuge the obtained precipitate repeatedly and wash it with deionized water, and dry it at 60° C. for 12 hours to obtain the titanium nitride-based composite material sample 2.
实施例3Example 3
1)按5mg/cm2的比例，将氮化钛粉末均匀置放于聚四氟乙烯载架上；1) According to the ratio of 5mg/ cm2 , the titanium nitride powder is evenly placed on the polytetrafluoroethylene carrier;
2)将载架放置入装有15mL浓度为0.1mol/L的HNO3溶液的反应釜中，密封后置于烘箱，在180℃条件下，反应5h；2) Place the carrier into a reaction kettle filled with 15mL of HNO 3 solution with a concentration of 0.1mol/L, seal it, place it in an oven, and react at 180°C for 5h;
3)取出反应釜空冷到室温，将所得沉淀反复离心和去离子水冲洗，在60℃温度下干燥12h，获得氮化钛基复合材料样品3。3) Take out the reactor and cool it to room temperature in air, centrifuge the obtained precipitate repeatedly and wash it with deionized water, and dry it at 60° C. for 12 hours to obtain a titanium nitride-based composite material sample 3 .
图2所示为实施例3所得氮化钛基复合材料样品3的XRD结构表征图，由图2可以看出，所述纳米氮化钛基复合光催化材料由氮化钛(PDF卡片号38-1420)和二氧化钛(PDF卡片号21-1272)两相构成，氮化钛和二氧化钛两相重量比例分别为12％及88％。Fig. 2 shows the XRD structure characterization figure of embodiment 3 gained titanium nitride-based composite material sample 3, as can be seen from Fig. 2, described nano-titanium nitride-based composite photocatalytic material is made of titanium nitride (PDF card number 38 -1420) and titanium dioxide (PDF card No. 21-1272) two-phase composition, the two-phase weight ratio of titanium nitride and titanium dioxide is 12% and 88% respectively.
图3所示为实施例3所得氮化钛/二氧化钛复合材料的TEM图，由图3可以看出，氮化钛基复合材料为在氮化钛表面原位生长二氧化钛，进而获得以氮化钛为基的复合材料。Figure 3 shows the TEM image of the titanium nitride/titanium dioxide composite material obtained in Example 3. As can be seen from Figure 3, the titanium nitride-based composite material grows titanium dioxide in situ on the titanium nitride surface, and then obtains titanium nitride Based composite material.
实施例4Example 4
1)按5mg/cm2的比例，将氮化钛粉末均匀置放于聚四氟乙烯载架上；1) According to the ratio of 5mg/ cm2 , the titanium nitride powder is evenly placed on the polytetrafluoroethylene carrier;
2)将载架放置入装有15mL浓度为0.01mol/L的HF溶液的反应釜中，密封后置于烘箱，在180℃条件下，反应1.5h；2) Place the carrier into a reaction kettle filled with 15mL of HF solution with a concentration of 0.01mol/L, seal it and place it in an oven, and react at 180°C for 1.5h;
3)取出反应釜空冷到室温，将所得沉淀反复离心和去离子水冲洗，在60℃温度下干燥12h，获得氮化钛基复合材料样品4。3) Take out the reactor and cool it to room temperature in air, centrifuge the obtained precipitate repeatedly and wash it with deionized water, and dry it at 60° C. for 12 hours to obtain a titanium nitride-based composite material sample 4 .
实施例5Example 5
1)按5mg/cm2的比例，将氮化钛粉末均匀置放于聚四氟乙烯载架上；1) According to the ratio of 5mg/ cm2 , the titanium nitride powder is evenly placed on the polytetrafluoroethylene carrier;
2)将载架放置入装有15mL浓度为1.0mol/L的HNO3溶液的反应釜中，密封后置于烘箱，在180℃条件下，反应2h；2) Put the carrier into a reaction kettle filled with 15mL of HNO 3 solution with a concentration of 1.0mol/L, seal it and place it in an oven, and react for 2 hours at 180°C;
3)取出反应釜空冷到室温，将所得沉淀反复离心和去离子水冲洗，在60℃温度下干燥12h，获得氮化钛基复合材料样品5。3) Take out the reaction kettle and air cool to room temperature, centrifuge the obtained precipitate repeatedly and wash it with deionized water, and dry it at 60° C. for 12 hours to obtain a titanium nitride-based composite material sample 5 .
表1实施例1-5所得样品中两相比例Two-phase ratio in the obtained sample of table 1 embodiment 1-5
实施例结果表明，本发明采用气相水热的手段对氮化钛基体进行可控的氧化，在其表面原位生长二氧化钛，进而获得以氮化钛为基的复合材料。通过控制制备工艺(反应时间和/或溶液浓度)，可以获得不同两相比例的复合材料，是一种简单、高效的复合合成方法，特别是该方法获得的复合材料界面接触良好，保证了两相间的载流子的有效传输，同时解决了传统复合方法需要高温煅烧的难题。The results of the examples show that the present invention uses gas-phase hydrothermal means to oxidize the titanium nitride matrix in a controlled manner, grows titanium dioxide on its surface in situ, and then obtains a titanium nitride-based composite material. By controlling the preparation process (reaction time and/or solution concentration), composite materials with different two-phase ratios can be obtained, which is a simple and efficient composite synthesis method, especially the composite material interface contact obtained by this method is good, ensuring that the two phases The effective transport of carriers between phases also solves the problem of high-temperature calcination required by traditional composite methods.
Claims (8)
- It is 1. a kind of to prepare the method for nitrogenizing titanium matrix composite, it is characterised in that：The method uses gas phase hydrothermal method Nitridation Titanium base is aoxidized, titanium dioxide is grown in its surface in situ, so as to obtain by titanium nitride and titanium dioxide The nitridation titanium matrix composite of the phase composition of titanium two.
- It is 2. according to claim 1 to prepare the method for nitrogenizing titanium matrix composite, it is characterised in that：The method Specifically include following steps：(1) nitridation Titanium base is uniformly positioned on polytetrafluoroethylene (PTFE) carrier；(2) carrier that will be loaded with nitridation Titanium base is positioned in the reactor with polytetrafluoroethyllining lining, is reacted Kettle is built with HNO3Or HF solution, reactor is placed in baking oven after sealing, reacted under the conditions of 150-180 DEG C 1-12h；(3) take out reactor and be air cooled to room temperature, after gained is precipitated through centrifugation and deionized water rinsing, at 60 DEG C Under the conditions of dry 10-24h, that is, obtain the nitridation titanium matrix composite.
- It is 3. according to claim 2 to prepare the method for nitrogenizing titanium matrix composite, it is characterised in that：Step (1) In, the nitridation Titanium base is film-form or powdered titanium nitride material.
- It is 4. according to claim 2 to prepare the method for nitrogenizing titanium matrix composite, it is characterised in that：Step (2) In, the HNO3Or the concentration of HF solution is 0.01-1.0mol/L.
- It is 5. according to claim 2 to prepare the method for nitrogenizing titanium matrix composite, it is characterised in that：Step (2) In, the nitridation Titanium base being placed in reactor on carrier is located at HNO3Or the top of HF liquid level of solution.
- It is 6. according to claim 2 to prepare the method for nitrogenizing titanium matrix composite, it is characterised in that：Prepare nitrogen During change titanium matrix composite, by controlling HNO3Or HF solution concentration and the reaction time to regulate and control The two-phase proportion of titanium nitride and titanium dioxide in titanium matrix composite must be nitrogenized.
- It is 7. according to claim 6 to prepare the method for nitrogenizing titanium matrix composite, it is characterised in that：Prepare nitrogen During change titanium matrix composite, the HNO3Or the concentration of HF solution is higher, dioxy in gained composite Change titanium proportion bigger；Reaction time is more long, and titanium dioxide proportion is bigger in gained composite.
- It is 8. according to claim 1 to prepare the method for nitrogenizing titanium matrix composite, it is characterised in that：Gained nitrogen Change in titanium matrix composite, the two-phase proportion scope of titanium nitride and titanium dioxide is 0-100%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312218A (en) * | 2001-03-23 | 2001-09-12 | 中国科学院上海硅酸盐研究所 | Titania nitriding process for preparing nanometer titanium nitride powder |
| CN102357365A (en) * | 2011-09-07 | 2012-02-22 | 复旦大学 | Preparation method for titanium oxynitride photocatalyst |
| CN102962089A (en) * | 2012-11-26 | 2013-03-13 | 杭州电子科技大学 | A method for preparing nitrogen-doped rutile TiO2 selective photocatalyst |
| CN103848457A (en) * | 2012-11-29 | 2014-06-11 | 中国科学院合肥物质科学研究院 | Nitrogen-doped anatase crystal form titanium dioxide nanopowder and preparation method thereof |
| CN104261466A (en) * | 2014-07-30 | 2015-01-07 | 深圳孔雀科技开发有限公司 | Method for preparing black titanium dioxide by using hydrothermal synthesis method |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312218A (en) * | 2001-03-23 | 2001-09-12 | 中国科学院上海硅酸盐研究所 | Titania nitriding process for preparing nanometer titanium nitride powder |
| CN102357365A (en) * | 2011-09-07 | 2012-02-22 | 复旦大学 | Preparation method for titanium oxynitride photocatalyst |
| CN102962089A (en) * | 2012-11-26 | 2013-03-13 | 杭州电子科技大学 | A method for preparing nitrogen-doped rutile TiO2 selective photocatalyst |
| CN103848457A (en) * | 2012-11-29 | 2014-06-11 | 中国科学院合肥物质科学研究院 | Nitrogen-doped anatase crystal form titanium dioxide nanopowder and preparation method thereof |
| CN104261466A (en) * | 2014-07-30 | 2015-01-07 | 深圳孔雀科技开发有限公司 | Method for preparing black titanium dioxide by using hydrothermal synthesis method |
Non-Patent Citations (2)
| Title |
|---|
| PORUN LIU ET AL.: "A Facile Vapor-Phase Hydrothermal Method for Direct Growth of Titanate Nanotubes on a Titanium Substrate via a Distinctive Nanosheet Roll-Up Mechanism", 《JOURNAL OF THE AMERICAN CHEMICAL SOCIETY》 * |
| PORUN LIU ET AL.: "Vapor-Phase Hydrothermal Transformation of HTiOF 3 Intermediates into {001} Faceted Anatase Single-Crystalline Nanosheets", 《SMALL》 * |
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