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HPHT Synthesis And Characterization Of CBN-based Composite Materials

Posted on:2021-02-01Degree:DoctorType:Dissertation
Country:ChinaCandidate:D L ChuFull Text:PDF
GTID:1361330623977316Subject:Condensed matter physics
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cBN is synthetic crystal with hardness next to diamond.Although the hardness of cBN is lower than that of diamond,its thermal stability is higher than that of diamond.In addition,PcBN tool has an absolute advantage in cutting iron-based metal materials,because in the high temperature environment of cutting,iron-based metal is easy to react with diamond and corrode diamond tool,while cBN has a great chemical inertia to iron-based metal.However,compared with diamond,cBN is more difficult to synthesize large single crystal.Most of the researchers synthesized cBN particles in micron size.Therefore,how to bond cBN particles in micron size and the bonding effect determines the properties of cBN based composite materials.Al2O3 is a kind of oxide with high hardness,and Al2O3 is stable under HPHT conditions.A series of cBN-Al2O3 composites were synthesized under HPHT conditions.Al reacts with cBN and forming AlN under HPHT conditions.A series of cBN?Al?-Al2O3 composites were synthesized under HPHT conditions after cBN particles were coated with Al film.B2O3 is the oxide of cBN,and cBN is superhard material with hardness next to diamond.What about the hardness and other properties of B2O3 after HPHT treatment?Through literature search,the research reported in this area is still very little.Therefore,we have done a series of research on B2O3 under HPHT conditions.Through the research,this thesis obtains the following findings and conclusions.1.We synthesized cBN-Al2O3 composites in NaCl environment under HPHT conditions,and we characterized the thermogravimetry and Vickers hardness of cBN-Al2O3 composites.The results show that the porosity of cBN-Al2O3 composites decreases with the increase of Al2O3.Al2O3 inhibited the appearance of porosity between cBN particles,and Al2O3 as support material makes it possible to form chemical bond at the tip of cBN particles.The oxidation resistance of cBN-Al2O3composites reaches 1300?,which is 200?higher than that of raw cBN powder and100?higher than that of cBN+0 vol%Al2O3.The hardness of cBN+30 vol%Al2O3composite is 21.6 GPa.A new method of indirectly controlling the porosity of cBN-Al2O3 composites by adjusting the content of NaCl was proposed.2.A series of cBN?Al?-Al2O3 composites were synthesized under HPHT conditions of the pressure of 5.0 Gpa and temperature of 1200-1500?after coating cBN particles with Al.Under the pressure of 5.0 Gpa and the temperature of1200-1500?,NaCl began to infiltrate into the cBN?Al?-Al2O3 composites,and cBN does not change into hBN.After XRD characterization of cBN?Al?-Al2O3 composites,we found that Al reacted with cBN particles under HPHT conditions and generated AlN.AlN phase as bridge phase connects cBN phase and Al2O3 phase.Under HPHT experiment conditions,the process can be divided into two parts.On the one hand,Al film reacts with cBN to form AlN,on the other hand,Al film reacts with oxygen which exist in the pores between cBN particles to form Al2O3.The hardness of cBN?Al?-Al2O3 composites is 37.5%higher than that of cBN-Al2O3 composites.The starting oxidation temperature of cBN to B2O3 in cBN?Al?-Al2O3 composites is about50?lower than that of cBN-Al2O3 composites.In addition,the micro amount of NaCl in cBN?Al?-Al2O3 composites increase the density of cBN?Al?-Al2O3composites.The porosity of cBN?Al?-Al2O3 composites can be indirectly controlled by controlling the content of NaCl in the samples.3.We treated glassy B2O3 under HPHT conditions and obtained the phase diagram of B2O3.We studied the phase diagram of B2O3 systematically,the phase diagram of B2O3 is mainly divided into three parts:low pressure?-B2O3 crystal phase,high pressure?-B2O3 crystal phase and high temperature vitreous B2O3 phase.We found that in the low-temperature region of B2O3 phase diagram,the color,toughness and hardness of B2O3 changed obviously due to the grain size of B2O3 decreased to nanometer level,and we marked this low-temperature region in B2O3 phase diagram.The hardness of?-B2O3 which synthesized at 5.5 Gpa and 450?reached 13.9 GPa,this is consistent with the hardness of 16?5?GPa of?-B2O3 previously reported.At last,we characterized the B2O3 after HPHT treatment by Raman spectrum.Raman spectrum of B2O3 indicate that boroxol rings only exist in vitreous B2O3 transformed from?-B2O3 phase but not in vitreous B2O3 transformed from?-B2O3 phase.This occurs because?-B2O3 phase is composed of ribbons formed by planar BO3 triangles and?-B2O3 phase is composed of BO4 tetrahedrons.As the temperature increases to the glass transition temperature,the ribbon chains gradually break up and the planar BO3 triangles form the more stable boroxol rings.The?-B2O3 phase is composed of BO4 tetrahedrons;therefore,no boroxol rings are produced.In conclusion,cBN-Al2O3 composites and cBN?Al?-Al2O3 composites were successfully synthesized by HPHT method.Under HPHT conditions,Al2O3 can fill the pores between cBN particles and support cBN particles.The properties of cBN-Al2O3 composite and cBN?Al?-Al2O3 composite were fully analyzed and discussed by means of XRD,SEM,Vickers hardness and TGA.Compared with cBN-Al2O3 composite,the Vickers hardness of cBN?Al?-Al2O3 composite is increased by 37.5%,and its thermal stability is reduced by 50?.At last,we obtained the phase diagram of B2O3 which is the oxide of cBN,and studied the hardening mechanism of B2O3 and the formation mechanism of boroxol rings.This paper provides an important reference value for the further study of cBN-based composite materials under HPHT conditions.
Keywords/Search Tags:HPHT, superhard materials, cBN-based composite materials, Al2O3, B2O3, hardness, thermogravimetry
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