Effects Of Different Pretreatment Methods On The Composition And Structure Of Biphasic Calcium Phosphate Material From Marine Fish Bone

ObjectBy comparing the effects of different pretreatment methods on HA / ?-TCP biphasic calcium phosphate(BCP)from salmon bone,the treatment methods and conditions were selected that can not only improve the relative content of ?-TCP,but also optimize the microstructure.On this basis,it can be applied to different kinds of fish bones to verify the universality of this method,and provide the basis for the modification of BCP materials from fish bones in the future.MethodExperiment One The effect of organics removal of different pretreatment methods and their influence on the inorganic composition and structure of the salmon-bone-derived BCP material.With the salmon bone as the raw material,reveal the organics removal effect of pretreatment methods of hydrogen peroxide solutions,methanol/chloroform solution,high temperature calcination and blank pretreatment through general observation,SEM and Fourier transform infrared(FTIR),etc.Then calcinate the treated fishbone with high temperature to get the BCP material,and demonstrate the effect of different pretreatment methods on the inorganic composition and microstructure of the fishbone-derived BCP material through SEM,XRD,MIP and so on.Experiment Two The effect of different pretreatment time of the hydrogen peroxide solution on the composition and structure of the salmon-bone-derived BCP material.With the salmon bone as the raw material,pretreat the hydrogen peroxide solution for various times,then make the BCP material through high temperature calcination and reveal its composition and microstructure through SEM,XRD,MIP and so on.Experiment Three The effect of the pretreatment method of the hydrogen peroxide solution on the composition and structure of the BCP material derived from marine fishbone of different kinds.Taking the bone of the sole fish,butterfish and yellow croaker as the raw material,pretreat the bone with 30% hydrogen peroxide solution or skip the step,then make the BCP material from bones of various kinds of fish through high temperature calcination.Demonstrate the composition and microstructure of the BCP material made from bones of various kinds of fish through general observation,SEM,XRD,etc.ResultsExperiment One From the general observation and SEM observation and the FTIR analysis,it can be seen that the organic characteristic functional groups contained in the untreated salmon bone such as a large amount of collagen and fat has basically disappeared after the 900? high temperature calcination;the hydrogen peroxide solution and methanol/chloroform solution can remove a majority of organics except for a few remains.According to XRD analysis,pretreating with 30% hydrogen peroxide solution can obviously increase the relative content of ?-TCP in the salmon-bone-derived BCP material while the methanol/chloroform solution does not have such effect.The results of SEM and MIP show that the hydrogen peroxide solution didn't obviously change the grain size of the BCP material but can increase the number of micropore and the surface area of the material;the BCP material pretreated with the methanol/chloroform solution has no obvious change in its microstructure;the twice calcination,however,enlarges the grain size,increases the diameter of the micropore and decreases the surface area.In a word,the hydrogen peroxide solution may be a pretreatment solution that can increase the relative content of ?-TCP in the fishbone-derived BCP material and can be benefit to its microstructure.Experiment Two According to the XRD analysis on the BCP material made from the Salmon bone,the relative content of TCP in the material first increases than decreases as the time of the hydrogen peroxide solution treatment increases and reaches the peak at 16 h.The change of the rate of calcium to phosphorus is the same as the result of XRD.The ICP also shows a small amount of metal elements which has not been affected by the pretreatment time of the hydrogen peroxide solution.The results of the SEM and MIP show that as the time of pretreatment increases,the grain size of the BCP material does not have obvious change;the large pores first gather than disperse;the diameter of the micropore has no obvious change while its number increases and reached its peak at 16h;the surface area also expands as the time increases.So,16 h may be the best pretreatment time for the hydrogen peroxide solution.Experiment Three Through the analysis on XRD and FTIR,we find 3 kinds of marine bone that can produce BCP,among which the relative content of ?-TCP in the sole fish is the highest of 31%.Different kinds of fish bone show different changes in the relative content of TCP after being pretreated by the hydrogen peroxide solution,among which the change of the yellow croaker is the largest with an increase of 100%.The BCP material made from the three fish bones also contains a small amount of CO32-and tracemental elements.The results of SEM and MIP shows that the grain size of the sole fish is much smaller than that of the butterfish and yellow croaker,and that the 30% hydrogen peroxide solution has no obvious effect on the grain size of the three kinds of fish bones.The effect of the solution on the micropore structure of the 3 fish bones mainly reveals on the increase of the number of the micropore and the expansion of the surface area in different degrees.So,the pretreatment method of the hydrogen peroxide solution can be used on various fishbone-derived BCP material to change its composition and structure.ConclusionsBy comparing the effects of different pretreatment methods on the composition and structure of salmon bone,we selected hydrogen peroxide solution as pretreatment method,which can not only significantly improve the relative content of ?-TCP in BCP material from salmon bone,but also increase the number of micropores,increase the specific surface area and optimize the microstructure.On this basis,the effects of different hydrogen peroxide treatment time on the composition and structure of BCP from salmon bone were studied.It is found that the highest relative content of ?-TCP,the number of micropores and the specific surface area can be obtained after treatment with hydrogen peroxide solution for 16 hours,which achieves the best treatment effect.Based on this,we used hydrogen peroxide solution to pretreat different kinds of BCP materials from marine fish bones,and found that for Longli,pomfret and yellow croaker bones,it can also increase the relative content of ?-TCP,the number of micropores and the specific surface area of BCP materials.The results show that the effect of hydrogen peroxide solution on the relative content of ?-TCP and the optimization of microstructure are suitable for many kinds of fish bones,which provides some basis for the modification of BCP materials from fish bones in the future.