阅读说明：本技术 一种高通用性耐高温的磷酸铝盐胶黏剂及其制备方法 (A kind of high universalizable phosphalugel adhesive resistant to high temperature and preparation method thereof ) 是由 刘家臣 张芳芳 郭安然 刘子浩 曹成昊 于 2018-05-22 设计创作，主要内容包括：一种高通用性耐高温的磷酸铝盐胶黏剂及其制备方法,是应用于氧化物陶瓷、非氧化物陶瓷以及陶瓷基复合材料的粘接,这种胶黏剂是以磷酸二氢铝为基体,以硅粉和碳化硼粉为改性填料,固化温度低,可在常低温下固化,具有“固化后无需后处理高低温通用”的特点,且在高温900℃以上时,剪切强度大,力学性能和耐热性能优良；该胶黏剂粘稠度低,易于搅拌及操作,能够粘接氧化物陶瓷、非氧化物陶瓷及陶瓷基复合材料；该方法制备工艺简单,易于操作。(A kind of high universalizable phosphalugel adhesive resistant to high temperature and preparation method thereof, it is the bonding applied to oxide ceramics, non-oxide ceramics and ceramic matric composite, this adhesive is using aluminium dihydrogen phosphate as matrix, using silicon powder and boron carbide powder as modified filler, solidification temperature is low, can be in normal curing at low temperatures, have the characteristics that " general without post-processing high/low temperature after solidification ", and at 900 DEG C of high temperature or more, shear strength is big, mechanical property and fine heat-resisting performance；The adhesive viscosity is low, is easy to stir and operate, can be bonded oxide ceramics, non-oxide ceramics and ceramic matric composite；This method preparation process is simple, easily operated.)

1. a kind of preparation method of high universalizable phosphalugel adhesive resistant to high temperature, it is characterised in that: be specifically according to following What step carried out:

(1) the concentrated phosphoric acid aqueous solution, 30 parts of deionized waters and 70-85 parts that 100 parts of mass concentrations are 85% are weighed according to parts by weight Aluminium-hydroxide powder；

(2) phosphoric acid solution is uniformly mixed with deionized water, is diluted to the phosphate aqueous solution that mass concentration is 65%；

(3) phosphoric acid solution in step (2) is placed in water-bath and keeps the temperature 5min-10min, controlled at 80 DEG C -90 DEG C, While being stirred with blender, it is slowly added to the aluminium hydroxide of step (1) weighing, continues the mechanical stirring mixed solution, 20min-30min is reacted, certain viscosity aluminium dihydrogen phosphate matrix body is obtained, controls its viscosity not higher than 3000mPas；

(4) the aluminium dihydrogen phosphate matrix body, 1-20 parts of silicon powders and 1-20 parts that 100 parts of steps (3) obtain are weighed according to parts by weight Boron carbide powder；

(5) silicon powder and boron carbide powder are uniformly mixed, obtain modified filler；

(6) modified filler in step (5) is added in the aluminium dihydrogen phosphate matrix body of step (4), is uniformly mixed；

(7) step (6) adhesive is put into vacuum tank and is vacuumized 10 minutes, adhesive surface has bubble suction and gas The additive powder for not being dissolved in solution wrapped up in bubble can also be brought to surface, futher stir, repeat vacuum, until Additive powder is completely dissolved in adhesive to get a kind of phosphalugel adhesive of the normal low-temperature setting of wide temperature range；Wherein phosphoric acid The mass ratio of aluminum dihydrogen and modified filler is 100:10-30, and curing time is 5-10h at room temperature；

(8) thickness control of the adhesive layer of step (7) high temperature resistant phosphalugel adhesive, which is 150-250 μm, is advisable, in room temperature and Solidify under the conditions of constant compression condition (0.75MPa).

Technical field

The present invention relates to a kind of preparation method field of phosphalugel adhesive, be suitable for aerospace, nuclear engineering and its In superhigh temperature resistant structural material applied in his various energy industry fields more particularly to a kind of high universalizable phosphorus resistant to high temperature Sour aluminium salt adhesive and preparation method thereof.

Background technique

The use of refractory ceramics and ceramic matric composite be unable to do without high-temperature Resistance Adhesives, and high-temperature resistant result is good and applies High temperature adhesive easy to operate has in energy fields such as the aerospace fields and nuclear engineering for possessing high technology content lifts foot The effect of weight.Although being in fact, high-temperature Resistance Adhesives can be used for preparing high temperature complex components [[i]] Reach the high intensity and stability [[ii]] of prepared complex components, which also needs high-temperature heating [[iii]], Therefore, high-temperature Resistance Adhesives need to have room temperature or the cured advantage of lower temperature and high-temperature stability.Adhesive it is normal low Warm solidification effect may be implemented disposably to connect, greatly simplifie operating procedure；The heat-resisting quantity of adhesive can guarantee it Safety in utilization [[iv]] in a high temperauture environment.

The normal low temperature difficulty solidification of the high-temperature Resistance Adhesives of existing preparation, or often after low-temperature setting at 900 DEG C of high temperature or more power It learns performance and heat resistance is poor, it is difficult to it is common to the bonding of oxide ceramics, non-oxide ceramics and ceramic matric composite, and Preparation process is complicated.

Major part Experimental report only has studied adhesive to single oxide or single non-oxide ceramics and pottery at present The bond effect of porcelain based composites seldom has been reported that studying one kind is suitable for a variety of high-temperature structural ceramics and ceramic base composite wood The high universalizable adhesive of material, therefore studying high versatility, normal low-temperature setting and heat-resist high-temperature Resistance Adhesives is very It is necessary.

Bibliography

[] Wang M C, Liu J C, Du H Y, et al. A New Practical Inorganic Phosphate Adhesive Applied under Both Air and Argon Atmosphere [J]. Journal of Alloys and Compounds, 2014, 617: 219-221.

[] Wang M C, Hu X X, Xu X Q, et al. A User-Friendly Heat-Resistant Modified Polymer-Based Adhesive for Joining and Repair of Carbon/Carbon Composites [J]. Materials and Design, 2015, 86: 709-713.

[] Wang M C, Tao X, Xu X Q, et al. High-Temperature Bonding Performance of Modified Heat-Resistant Adhesive for Ceramic Connection, Journal of Alloys and Compounds [J]. 2016, 663: 82-85.

[] Jin K K, Dai G L. Characteristics of Plasma Surface Treated Composite Adhesive Joints at High Environmental Temperature [J]. Composite Structures, 2002, 57: 37-46。

Summary of the invention

For problem of the existing technology, a kind of high universalizable of present invention phosphalugel adhesive resistant to high temperature and its system Preparation Method, using aluminium dihydrogen phosphate as matrix, using silicon powder and boron carbide powder as modified filler, solidification temperature is low, can normal low-temperature setting, And at 900 DEG C of high temperature or more, shear strength is big, mechanical property and fine heat-resisting performance；The simple process of preparation method, is easy to Operation.

A kind of high universalizable phosphalugel adhesive resistant to high temperature and preparation method thereof, the specific steps are as follows:

(1) the concentrated phosphoric acid aqueous solution, 30 parts of deionized waters and 70-85 parts that 100 parts of mass concentrations are 85% are weighed according to parts by weight Aluminium-hydroxide powder；

(2) phosphoric acid solution is uniformly mixed with deionized water, is diluted to the phosphate aqueous solution that mass concentration is 65%；

(3) phosphoric acid solution in step (2) is placed in water-bath and keeps the temperature 5min-10min, controlled at 80 DEG C -90 DEG C, While being stirred with blender, it is slowly added to the aluminium hydroxide of step (1) weighing, continues the mechanical stirring mixed solution, 20min-30min is reacted, certain viscosity aluminium dihydrogen phosphate matrix body is obtained, controls its viscosity not higher than 3000mPas；

(4) the aluminium dihydrogen phosphate matrix body, 1-20 parts of silicon powders and 1-20 parts that 100 parts of steps (3) obtain are weighed according to parts by weight Boron carbide powder；

(5) silicon powder and boron carbide powder are uniformly mixed, obtain modified filler；

(6) modified filler in step (5) is added in the aluminium dihydrogen phosphate matrix body of step (4), is uniformly mixed；

(7) step (6) adhesive is put into vacuum tank and is vacuumized 10 minutes, adhesive surface has bubble suction and gas The additive powder for not being dissolved in solution wrapped up in bubble can also be brought to surface, futher stir, repeat vacuum, until Additive powder is completely dissolved in the high temperature resistant phosphalugel adhesive in adhesive to get a kind of normal low-temperature setting of high universalizable； Wherein the mass ratio of aluminium dihydrogen phosphate and modified filler is 100:10-30, and curing time is 5-10h at room temperature；

(8) thickness control of the adhesive layer of step (7) high temperature resistant phosphalugel adhesive, which is 150-250 μm, is advisable, in room temperature and Solidify under the conditions of constant compression condition (0.75MPa).

A kind of high universalizable phosphalugel adhesive resistant to high temperature be applied to oxide ceramics, non-oxide ceramics and The bonding of ceramic matric composite, this adhesive are using aluminium dihydrogen phosphate as matrix, are that modification is filled out with silicon powder and boron carbide powder Material, solidification temperature is low, normal temperature solidified, has the characteristics that " general without post-processing high/low temperature after solidification ".And at 900 DEG C of high temperature When above, shear strength is big (as shown in the table), mechanical property and fine heat-resisting performance.The adhesive viscosity is low, is easy to stir It mixes and operates, oxide ceramics, non-oxide ceramics and ceramic matric composite can be bonded.The technique of preparation method of the present invention Simply, easily operated.

Specific embodiment

The present invention is described in further details below with reference to specific embodiment.