CN101186474A - Cement-based composite wave-absorbing material doped with nano-titanium oxide and its preparation method - Google Patents
Cement-based composite wave-absorbing material doped with nano-titanium oxide and its preparation method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
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Abstract
一种掺纳米氧化钛的水泥基复合吸波材料及制备方法,该复合吸波材料由纳米氧化钛、分散剂、硅酸盐水泥、和水组成,分散体系包括分散剂六偏磷酸钠和水,分散剂六偏磷酸钠占分散体系重量的质量百分比为0.3%-0.7%、水与干物料的比值也就是水灰比在0.32-0.38之间。制备步骤为:a.超声波制备纳米氧化钛的悬浮液,b.掺纳米氧化钛的水泥基复合吸波材料的制备方法。本发明在传统水泥材料中掺入少量的纳米氧化钛吸波剂,使水泥基复合材料具有较好的吸波性能和力学性能,其经济成本增加不多,制备工艺简单可行。
A cement-based composite wave-absorbing material doped with nano-titanium oxide and a preparation method thereof, the composite wave-absorbing material is composed of nano-titanium oxide, a dispersant, Portland cement, and water, and the dispersion system includes the dispersant sodium hexametaphosphate and water The mass percentage of the dispersant sodium hexametaphosphate to the weight of the dispersion system is 0.3%-0.7%, and the ratio of water to dry material, that is, the water-cement ratio is between 0.32-0.38. The preparation steps are: a. preparing nano titanium oxide suspension by ultrasonic wave; b. preparation method of cement-based composite wave-absorbing material mixed with nano titanium oxide. The invention mixes a small amount of nano-titanium oxide wave-absorbing agent into the traditional cement material, so that the cement-based composite material has better wave-absorbing performance and mechanical performance, the economic cost is not much increased, and the preparation process is simple and feasible.
Description
技术领域technical field
本发明属于建筑功能材料技术领域。The invention belongs to the technical field of building functional materials.
背景技术Background technique
水泥基复合吸波材料是在水泥或混凝土中掺入吸波剂而具有吸收电磁波功能的一类新型材料。在民用方面,它即可以用来屏蔽电磁波对人体的辐射,达到净化电磁波污染环境的目的;还可以用来防止计算机中心的数据泄漏,起到保密作用。在军事上,水泥基复合吸波材料可以起到干扰雷达探测目标、减弱回波信号,使雷达无法探测到地面固定目标或探测精度明显降低,避免敌方的军事打击。用于民用建筑物的水泥基吸波材料对电磁波的反射率达5dB以上就具有实际使用价值,用于地面军事目标的水泥基吸波材料对雷达波的反射率超过7dB也具备工程应用价值。Cement-based composite wave-absorbing material is a new type of material that has the function of absorbing electromagnetic waves by mixing wave-absorbing agents into cement or concrete. In terms of civilian use, it can be used to shield the radiation of electromagnetic waves on the human body to achieve the purpose of purifying the environment polluted by electromagnetic waves; it can also be used to prevent data leakage in the computer center and play a role in keeping secrets. In the military, cement-based composite absorbing materials can interfere with radar detection targets and weaken echo signals, so that radars cannot detect fixed targets on the ground or the detection accuracy is significantly reduced, avoiding enemy military strikes. Cement-based absorbing materials used for civil buildings have practical value for electromagnetic waves with a reflectivity of more than 5dB, and cement-based absorbing materials for ground military targets with a reflectivity of more than 7dB for radar waves also have engineering application value.
国外在上世纪90年代初就开始研究电磁屏蔽水泥混凝土,其中以D.D.L.Chung为首的科研组研究了把细碳丝、钢回形针、胶状石墨、焦碳粉和不锈钢纤维分别掺入水泥中制成的水泥基复合材料,这种水泥基复合材料在1.5GHz以内的屏蔽效能一般可以达到40dB左右,但反射衰减只有2-4dB。近年来国内有些学者也开展了这方面的研究工作,如杨海燕等人研究了掺钢纤维的水泥砂浆,在2-18GHz频率范围内,该水泥砂浆试样的吸收率为4dB的带宽可达15.28GHz,最大吸收率为9.8dB;赵彦波等人研究了掺有发泡型聚苯乙烯(EPS)的水泥基多孔复合吸波材料,当EPS的填充率(体积分数)为60%、样品厚度为20mm时,反射率小于-10dB的带宽达6GHz,在18GHz最小反射率达-15.27dB;许卫东等人研究了铁氧体吸波剂掺入到水泥砂浆中的吸波性能,当铁氧体掺量为33%(质量分数)、厚度为3mm时,在8-12GHz频段,最大反射率约7dB、最小反射率达15dB,说明铁氧体掺入到水泥砂浆中可提高材料的吸波性能。Foreign countries began to study electromagnetic shielding cement concrete in the early 1990s. Among them, the scientific research group headed by D.D.L. Chung studied the mixing of fine carbon wire, steel paper clip, colloidal graphite, coke powder and stainless steel fiber into cement. The cement-based composite material, the shielding effectiveness of this cement-based composite material within 1.5GHz can generally reach about 40dB, but the reflection attenuation is only 2-4dB. In recent years, some domestic scholars have also carried out research work in this area. For example, Yang Haiyan and others have studied cement mortar mixed with steel fibers. In the frequency range of 2-18GHz, the absorption rate of the cement mortar sample is 4dB and the bandwidth can reach 15.28 GHz, the maximum absorption rate is 9.8dB; Zhao Yanbo and others studied the cement-based porous composite absorbing material mixed with expanded polystyrene (EPS). When the filling rate (volume fraction) of EPS is 60% and the sample thickness is At 20mm, the bandwidth with a reflectivity less than -10dB reaches 6GHz, and the minimum reflectivity reaches -15.27dB at 18GHz; When the amount is 33% (mass fraction) and the thickness is 3mm, the maximum reflectance is about 7dB and the minimum reflectance is 15dB in the 8-12GHz frequency band, indicating that ferrite mixed into cement mortar can improve the absorbing performance of the material.
上述研究的水泥基屏蔽材料所屏蔽的电磁波频率几乎都在几十Hz到1-2GHz内,这些水泥基屏蔽材料主要用于防止电磁信号的泄露和外部的电磁干扰,其对电磁波的屏蔽效果较好,但对电磁波的吸收衰减和反射衰减较差;而所研究的水泥基吸波材料的吸波性能不理想,且掺有铁氧体吸波剂的水泥基复合材料的力学性能均有不同程度地降低,影响到实际应用。The frequency of electromagnetic waves shielded by the cement-based shielding materials studied above is almost in the tens of Hz to 1-2GHz. These cement-based shielding materials are mainly used to prevent the leakage of electromagnetic signals and external electromagnetic interference, and their shielding effect on electromagnetic waves is relatively low. Good, but the absorption attenuation and reflection attenuation of electromagnetic waves are poor; the absorbing properties of the cement-based absorbing materials studied are not ideal, and the mechanical properties of the cement-based composite materials mixed with ferrite absorbers are different. Reduced to a certain extent, affecting practical applications.
发明内容Contents of the invention
针对上述存在的问题,本发明的目的是以纳米氧化钛作为吸波剂,通过超声波分散使纳米氧化钛形成均匀的悬浮液,然后在机械搅拌下使纳米氧化钛的悬浮液和水泥混合均匀,经振动成型、养护制得水泥基复合吸波材料。In view of the above-mentioned problems, the object of the present invention is to use nano-titanium oxide as a wave-absorbing agent to form a uniform suspension of nano-titanium oxide through ultrasonic dispersion, and then mix the suspension of nano-titanium oxide with cement evenly under mechanical stirring. The cement-based composite wave-absorbing material is obtained through vibration molding and curing.
本发明和具体技术方案如下:The present invention and concrete technical scheme are as follows:
采用超声波分散技术和机械搅拌方法制得掺纳米氧化钛的水泥基复合吸波材料。其组成特征是:该复合吸波材料由纳米氧化钛、分散剂、硅酸盐水泥、和水组成,干物料为纳米氧化钛和硅酸盐水泥,纳米氧化钛占干物料的重量百分比为3%-7%、水泥占干物料的重量百分比为93%-97%。分散体系包括分散剂六偏磷酸钠和水,分散剂六偏磷酸钠占分散体系重量的质量百分比为0.3%-0.7%、水与干物料的比值也就是水灰比在0.32-0.38之间。The cement-based composite wave-absorbing material doped with nano-titanium oxide was prepared by ultrasonic dispersion technology and mechanical stirring method. Its composition features are: the composite wave-absorbing material is composed of nano-titanium oxide, dispersant, Portland cement, and water, the dry material is nano-titanium oxide and Portland cement, and the weight percentage of nano-titanium oxide in the dry material is 3 %-7%, and the weight percentage of cement in dry materials is 93%-97%. The dispersion system includes dispersant sodium hexametaphosphate and water, the mass percentage of the dispersant sodium hexametaphosphate to the dispersion system weight is 0.3%-0.7%, and the ratio of water to dry material, that is, the water-cement ratio is between 0.32-0.38.
该复合吸波材料的制备步骤和必要的工艺参数如下:The preparation steps and necessary process parameters of the composite wave-absorbing material are as follows:
1、超声波制备纳米氧化钛的悬浮液,1. Ultrasonic preparation of nano-titanium oxide suspension,
称取一定量的六偏磷酸钠分散剂,按0.3%-0.7%的分散体系重量的质量百分比计,溶于一定量的水中,保持分散体系的浓度在7.0%-10%之间,再称取3%-7%的纳米氧化钛,倒入上述溶液中,置于超声波分散仪中,超声分散20-30分钟,制得均匀的纳米氧化钛悬浮液。Weigh a certain amount of sodium hexametaphosphate dispersant, dissolve it in a certain amount of water according to the mass percentage of the dispersion system weight of 0.3%-0.7%, keep the concentration of the dispersion system between 7.0%-10%, and then weigh Take 3%-7% nano-titanium oxide, pour it into the above solution, place it in an ultrasonic disperser, and ultrasonically disperse for 20-30 minutes to prepare a uniform nano-titanium oxide suspension.
2、掺纳米氧化钛的水泥基复合吸波材料的制备方法2. Preparation method of cement-based composite wave-absorbing material doped with nano-titanium oxide
称取93%-97%的42.5#或32.5#、52.5#硅酸盐水泥和一定量的水,使水与干物料的比值即水灰比保持在0.32-0.38之间;把水泥置于搅拌灌中,开动搅拌,缓慢加入纳米氧化钛的悬浮液和水,搅拌3-5分钟后把混合料倒入钢模中,然后置于振动台上振动1-2分钟,抹平表面,在温度20℃-25℃、湿度为85-90%的条件下养护1天,拆模后继续在上述条件下养护28天,制得掺纳米氧化钛的水泥基复合吸波材料。Weigh 93%-97% of 42.5 # or 32.5 # , 52.5 # Portland cement and a certain amount of water, so that the ratio of water to dry material, that is, the water-cement ratio, is kept between 0.32-0.38; put the cement in the stirring Irrigate, start stirring, slowly add the suspension of nano-titanium oxide and water, stir for 3-5 minutes, pour the mixture into the steel mold, then place it on a vibration table and vibrate for 1-2 minutes, smooth the surface, Curing for 1 day under the conditions of 20°C-25°C and humidity of 85-90%, and continuing to cure under the above conditions for 28 days after removing the formwork, to obtain a cement-based composite wave-absorbing material doped with nano-titanium oxide.
本发明在传统水泥材料中掺入少量的纳米氧化钛吸波剂,使水泥基复合材料具有较好的吸波性能和力学性能,其经济成本增加不多,制备工艺简单可行。该水泥基复合吸波材料在8-26.5GHz频率范围内的反射率基本上小于7dB,最小反射率达17.37dB,反射率小于10dB的连续带宽达11GHz。表明该水泥基复合吸波材料在X(8-12.5GHz)、KU(12.5-18GHz)和K(18-26.5GHz)三个波段内具有较好的兼容吸波性能,实现了宽频吸波功效;同时其力学性能与水泥净浆相比提高了12.6%和19.1%,力学性能得到明显改善。The invention mixes a small amount of nano-titanium oxide wave-absorbing agent into the traditional cement material, so that the cement-based composite material has better wave-absorbing performance and mechanical performance, the economic cost is not much increased, and the preparation process is simple and feasible. The reflectivity of the cement-based composite wave-absorbing material in the frequency range of 8-26.5GHz is basically less than 7dB, the minimum reflectivity reaches 17.37dB, and the continuous bandwidth with the reflectivity less than 10dB reaches 11GHz. It shows that the cement-based composite absorbing material has good compatible absorbing performance in the three bands of X (8-12.5GHz), KU (12.5-18GHz) and K (18-26.5GHz), and realizes the effect of broadband absorbing ; At the same time, its mechanical properties are increased by 12.6% and 19.1% compared with the cement slurry, and the mechanical properties are obviously improved.
附图说明Description of drawings
图1实施例试样的反射率测试图;The reflectance test figure of Fig. 1 embodiment sample;
图2实施例试样的力学性能测试图。The mechanical performance test diagram of the sample of Fig. 2 embodiment.
具体实施例specific embodiment
实例1:Example 1:
1、超声波制备纳米氧化钛的悬浮液,1. Ultrasonic preparation of nano-titanium oxide suspension,
称取一定量的六偏磷酸钠分散剂按0.5%的分散体系重量的质量百分比计,溶于一定量的水中,保持分散体系的浓度在9.0%,再称取5%的纳米氧化钛,倒入上述溶液中,置于超声功率为150W、超声频率为40KHz的超声波分散仪中,超声分散25分钟,制得均匀的纳米氧化钛悬浮液。Take by weighing a certain amount of sodium hexametaphosphate dispersant according to the mass percentage of the dispersion system weight of 0.5%, dissolve it in a certain amount of water, keep the concentration of the dispersion system at 9.0%, then take by weighing 5% nano titanium oxide, pour into the above solution, placed in an ultrasonic disperser with an ultrasonic power of 150W and an ultrasonic frequency of 40KHz, and ultrasonically dispersed for 25 minutes to obtain a uniform nano-titanium oxide suspension.
2、掺纳米氧化钛的水泥基复合吸波材料的制备方法2. Preparation method of cement-based composite wave-absorbing material doped with nano-titanium oxide
称取95%的42.5#硅酸盐水泥和一定量的水,使水与干物料的比值即水灰比保持在0.35之间;把水泥置于搅拌灌中,开动搅拌,缓慢加入纳米氧化钛的悬浮液和水,搅拌3分钟后把混合料倒入截面为180mm×180mm、厚度为5-30mm的钢模中,然后置于振动台上振动1分钟,抹平表面,在温度20℃、湿度为90%的条件下养护1天,拆模后继续在上述条件下养护28天,制得掺纳米氧化钛的水泥基复合吸波材料。Weigh 95% of 42.5 # Portland cement and a certain amount of water, so that the ratio of water to dry material, that is, the water-cement ratio, is kept between 0.35; put the cement in the mixing tank, start stirring, and slowly add nano-titanium oxide After stirring for 3 minutes, pour the mixture into a steel mold with a cross-section of 180mm×180mm and a thickness of 5-30mm, then place it on a vibrating table and vibrate for 1 minute, and smooth the surface. It was cured for 1 day under the condition of 90% humidity, and continued to be cured under the above conditions for 28 days after removing the formwork to prepare a cement-based composite wave-absorbing material doped with nano-titanium oxide.
3.把养护28d后的试样测试其在8=26.5GHz频率范围内的反射率和其抗折与抗压强度,结果见图1和图2。3. Test the reflectivity and flexural and compressive strength of the sample after curing for 28 days in the frequency range of 8=26.5GHz. The results are shown in Figure 1 and Figure 2.
从图1中试样的反射率可以看出:水泥净浆试样的反射率均在6dB以上,而掺纳米氧化钛的水泥基复合吸波材料的反射率基本上在7dB以下,其中反射率小于10dB的连续带宽覆盖到13-24GHz,最小反射率出现在16.2GHz处,其值达17.37dB,体现出较好的宽频吸波性能。From the reflectance of the sample in Figure 1, it can be seen that the reflectance of the cement slurry sample is above 6dB, while the reflectance of the cement-based composite absorbing material doped with nano-titanium oxide is basically below 7dB. The continuous bandwidth of less than 10dB covers 13-24GHz, and the minimum reflectivity appears at 16.2GHz, with a value of 17.37dB, reflecting better broadband absorbing performance.
由图2中试样的力学性能可知:养护28d后试样的抗折和抗压强度分别比水泥净浆有不同程度的提高。From the mechanical properties of the samples in Figure 2, it can be seen that the flexural and compressive strengths of the samples after curing for 28 days are improved to varying degrees compared with the cement slurry.
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