CN106699162A - Arsenic-doped hydroxyapatite/calcium phosphate powder and preparation method thereof - Google Patents
Arsenic-doped hydroxyapatite/calcium phosphate powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses arsenic-doped hydroxyapatite/calcium phosphate powder and a preparation method thereof. The method comprises the steps of dropwise adding a mixed solution of a phosphorus source and an arsenic source into a calcium source solution for carrying out a reaction; after the reaction is finished, aging, centrifuging, drying and grinding to obtain arsenic-doped hydroxyapatite precursor powder; sintering the obtained arsenic-doped hydroxyapatite precursor powder to obtain the arsenic-doped hydroxyapatite/calcium phosphate powder. The preparation method provided by the invention is simple and efficient, and high in yield; the prepared arsenic-doped hydroxyapatite/calcium phosphate powder is good in dispersity.
Description
Technical field
The present invention relates to ion doping hydroxyapatite material field, and in particular to one kind mixes arsenic hydroxyapatite/phosphoric acid
Calcium powder body and preparation method thereof.
Background technology
Hydroxyapatite (HA) is the main inorganic composition of natural bone tissue, with good biocompatibility, frequently as
Bone renovating material implants.But the apatite in natural bone is not complete, but existing defects and replacement, F-、CO3 2-、
Mg2+、Si4+、Sr2+Plasma can mix apatite structure.Element is mixed into HA, nature bone component can not only be preferably simulated, also
The new functions of HA can be assigned.Biophasic calcium phosphate ceramic (BCP) often refers to the calcium phosphate material of different HA/ β-TCP ratios, and it has compared with HA more
Good solubility property.
The crystal of modification by ion-doping also in heat endurance, drops except being had a significant impact to mechanical property and physicochemical property
The aspects such as Xie Xing, surface-active and biological nature have very important change.Mixing silicon can effectively improve the bioactivity of HA, promote
Enter the Proliferation, Differentiation of Gegenbaur's cell;Mixing strontium can make the HA have more preferable mechanical property and biocompatibility;Mix human lymph node HA's
Antibiotic property and corrosion resistance, make HA have the effect of anti-inflammation;Mixing titanium can make HA with catalysis activity higher, rare earth doped
Element can make the HA have fluorescence property, can be applied to the biological applications such as fluorescence labeling and fluorescence probe.In the last few years, micro unit
The research of element doping HA achieves no small progress, and the doping of more and more element species makes the application of HA more and more extensive.
Arsenic is a kind of toxic element, but studies have found that, arsenious acid can suppress the proliferation activity of tumour cell and lure
The apoptosis of guided cell, Synergistic action is played by suppressing Tumor Angiongesis and suppressing telomerase activation.Micro amount of arsenic is mixed
HA, makes HA while having Bone Defect Repari and antitumaous effect, reduces the possibility of Patients with Osteosarcoma recurrence.But not yet there is research to report at present
Arsenic HA powder body materials are mixed in road, and can arsenic be mixed in HA, and what influence the incorporation of arsenic has on HA, and the incorporation of arsenic makes what HA specifically increased
Effect is planted, is all the problem for needing to further investigate and solve.
The content of the invention
In order to solve the above problems, it is an object of the invention to provide one kind mix arsenic hydroxyapatite/calcium phosphate powder and
Its preparation method, with obtain it is a kind of with good biological activity function biomaterial of calcium and phosphor, preparation mix arsenic hydroxyapatite/
Calcium phosphate powder yield is high, and good dispersion.
To achieve the above object, the present invention is realized using following technical scheme.
One kind mixes arsenic hydroxyapatite/calcium phosphate powder, and powder granule is rod-like structure long, and the length of rod-shaped particles long is
80~150nm, the width of rod-shaped particles long is 40~50nm;Mix in arsenic hydroxyapatite/calcium phosphate powder, arsenate instead of
Part phosphate radical, the doping of arsenic is 0.1~10wt%, preferably 3~10wt%;Mol ratio Ca:(P+As)=1.67.
A kind of above-mentioned method for mixing arsenic hydroxyapatite/calcium phosphate powder is prepared, is comprised the following steps:
(1) after by arsenic source solution and phosphorus source solution mixing and stirring, it is added drop-wise in calcium source solution;Continue after completion of dropping
Reaction, reaction is aged after terminating, is centrifuged, dries, grinding, and obtains mixing arsenic hydroxyapatite presoma powder;
(2) arsenic hydroxyapatite presoma powder will be mixed it will be placed in Muffle furnace and sinter, cooling will obtain described mixing arsenic hydroxyl phosphorus
Lime stone/calcium phosphate powder.
Further, in step (1), arsenic source solution is Na3AsO4Solution, concentration is 0.1mol/L.
Further, in step (1), phosphorus source solution is (NH4)3PO4·3H2O solution, concentration is 0.25mol/L.
Further, in step (1), the calcium source solution is Ca (NO3)2·4H2O solution, concentration is 0.5mol/L.
Further, in step (1), arsenic source solution is adjusted with the mixed mixed solution of phosphorus source solution with concentrated ammonia liquor
PH is to more than or equal to 10.
Further, in step (1), the calcium source solution uses concentrated ammonia liquor before mixed solution of the phosphorus source with arsenic source is added dropwise
Regulation pH adds dispersant and is disperseed to being more than or equal to 11, the addition of dispersant be calcium source solution 0.3~
0.4wt%.
Further, in step (1), the dispersant is polyethylene glycol, and the molecular weight of polyethylene glycol is 6000.
Further, in step (1), using peristaltic pump control, the speed of dropwise addition is 3~5mL/ to the speed of the dropwise addition
min。
Further, in step (1), the temperature of the reaction is 60~80 DEG C, and the time of reaction is 3~5h.
Further, in step (1), the time of the ageing is 24~48h.
Further, in step (1), the drying is in 50~60 DEG C of 12~24h of drying.
Further, in step (1), the sintering is to be warming up to 700~1100 DEG C with the heating rate of 5~10 DEG C/min
It is incubated 3h, preferably 900~1100 DEG C.
Further, in step (1), the cooling is to be down to normal temperature with the rate of temperature fall of 5~10 DEG C/min.
The present invention mixes arsenic hydroxyapatite/calcium phosphate powder, and arsenic can be mixed effectively in hydroxyapatite structure, and by adjusting
The incorporation of arsenic is saved, what sintering prepared different HA/ β-TCP ratios mixes arsenic biphasic calcium phosphate powder body material.
Compared with prior art, the present invention has advantages below and beneficial effect:
(1) to mix arsenic hydroxyapatite/calcium phosphate powder dispersity good for the present invention, is rod-like structure long, rod-shaped particles long
Average length reaches 80~150nm, and the width of rod-shaped particles long is 20~50nm;In mixing arsenic hydroxyapatite/calcium phosphate powder,
Arsenic amount is mixed for 0.1~10wt%.
(2) in preparation process of the present invention, the incorporation of arsenic is easily caused HA distortions of lattice, mix arsenic HA presoma powders it is sintered after
HA is set to be decomposed to form β-TCP;And the doping of arsenic is more, the β-TCP contents mixed in arsenic hydroxyapatite/calcium phosphate powder are got over
Greatly, therefore by adjust that the volume of arsenic can obtain different HA/ β-TCP two-phase ratios arsenic hydroxyapatite/calcium phosphate powder is mixed.
(3) using the antitumaous effect of arsenic, the present invention mixes arsenic hydroxyapatite/calcium phosphate powder body material and is expected to be applied to include
Bone tissue engineer and drug-loading system field.
(4) building-up process of the invention is simply efficient, and yield is high, and arsenic can be mixed effectively in hydroxyapatite structure, and
Prepared by sintering and mix arsenic hydroxyapatite/calcium phosphate powder.
Brief description of the drawings
Fig. 1 is the XRD for mixing arsenic hydroxyapatite presoma powder sample of the different arsenic doping amounts of embodiment 1;
Fig. 2 is the FTIR for the mixing arsenic hydroxyapatite presoma powder sample figures of the different arsenic doping amounts of embodiment 1;
Fig. 3 a are the SEM figures of sample 3 in embodiment 1;
Fig. 3 b are the EDS figures of sample 3 in embodiment 1;
Fig. 4 is the XRD for mixing arsenic hydroxyapatite/calcium phosphate powder sample of the different arsenic doping amounts of embodiment 2;
Fig. 5 is the XRD for mixing arsenic hydroxyapatite/calcium phosphate powder sample of the different arsenic doping amounts of embodiment 3;
Fig. 6 is the XRD for mixing arsenic hydroxyapatite/calcium phosphate powder sample of the different arsenic doping amounts of embodiment 4;
Fig. 7 is the FTIR for the mixing arsenic hydroxyapatite/calcium phosphate powder sample figures of the different arsenic doping amounts of embodiment 4.
Specific embodiment
The present invention is described in further detail with reference to specific embodiment, but protection scope of the present invention is not limited to
The content.
Embodiment 1
Prepare the doping of arsenic and mix arsenic for 0wt%, 0.1wt%, 0.5wt%, 1wt%, 3wt%, 5wt% and 10wt%
Hydroxyapatite presoma powder.
(1) by 0.1mol/L Na3AsO4(analysis is pure) solution and 0.25mol/L (NH4)3PO4·3H2O (analysis is pure) solution
Mixing and stirring, obtains phosphorus source/arsenic source mixed solution, and adjust mixed solution pH=10 with concentrated ammonia liquor;In 0.5mol/L Ca
(NO3)2·4H2The polyethylene glycol dispersant that 0.3wt% molecular weight is 6000,30min points of stirring are added in O (analysis is pure) solution
After dissipating uniformly, pH=11 is adjusted with concentrated ammonia liquor;
(2) in oil bath pan, control temperature for 80 DEG C, phosphorus source/arsenic source mixed solution is controlled into speed by peristaltic pump
5mL/min is added drop-wise to Ca (NO3)2·4H2In O (analysis is pure) solution, the amount of dropwise addition meets mol ratio Ca/ (P+As)=1.67;Drop
Add after finishing, the sustained response 3h at 80 DEG C, after reaction is aged 24h at room temperature after terminating, centrifuge washing, then at 60 DEG C
24h is dried, is ground after drying, obtain mixing arsenic hydroxyapatite presoma powder.
The different arsenic doping amounts for obtaining to mix arsenic hydroxyapatite presoma powder sample as shown in table 1.
Table 1 different arsenic doping amounts mix arsenic hydroxyapatite presoma powder
Sample | Mix arsenic amount (wt%) |
1 | 0 |
2 | 0.1 |
3 | 0.5 |
4 | 1 |
5 | 3 |
6 | 5 |
7 | 10 |
Fig. 1 is the XRD for mixing arsenic hydroxyapatite presoma powder sample of different arsenic doping amounts, as shown in figure 1, all
Sample all occurs in that the characteristic peak of hydroxyapatite, shows to be apatite material;As shown in Figure 1, with the increase of doping,
Sample diffraction peak broadens, and peak intensity weakens, crystallinity reduction.
Fig. 2 is the FTIR for the mixing arsenic hydroxyapatite presoma powder sample figures of different arsenic doping amounts, and appearance is shown in figure
The peak of hydroxyl, phosphate radical, carbonate and arsenate, illustrates to occur in that the official of hydroxyl, phosphate radical and arsenate in sample structure
Can roll into a ball, carbonate is wherein mainly based on Type B replacement.
Fig. 3 a scheme for the SEM of sample 3, and from Fig. 3 a, sample topography is rod long, 80~150nm, 20-50nm wide long;
Fig. 3 b are the EDS figures of sample 3, as shown in Figure 3 b, arsenic element are occurred in that in sample.
The X-ray fluorescence spectra test result such as table for mixing arsenic hydroxyapatite presoma powder sample of different arsenic doping amounts
Shown in 2.
Table 2 different arsenic doping amounts mix arsenic hydroxyapatite presoma powder X-ray fluorescence spectra test result
As shown in Table 2, the arsenic content in each sample is close with the incorporation value of theoretical arsenic, in illustrating that arsenic successfully mixes sample.
To sum up, arsenic is successfully entered hydroxyapatite lattice, and because arsenate is similar to phosphate radical, and arsenate is replacing phosphorus
The form of acid group enters in hydroxyapatite lattice structure.
Embodiment 2
700 DEG C of sintering prepare arsenic doping amount and mix arsenic hydroxyl phosphorus for 0wt%, 0.5wt%, 3wt%, 5wt% and 10wt%
Lime stone/calcium phosphate powder.
(1) by 0.1mol/L Na3AsO4(analysis is pure) solution and 0.25mol/L (NH4)3PO4·3H2O (analysis is pure) solution
Mixing and stirring, obtains phosphorus source/arsenic source mixed solution, and adjust mixed solution pH=10 with concentrated ammonia liquor;In 0.5mol/L Ca
(NO3)2·4H2The polyethylene glycol dispersant that 0.4wt% molecular weight is 6000,30min points of stirring are added in O (analysis is pure) solution
After dissipating uniformly, pH=11 is adjusted with concentrated ammonia liquor;
(2) in oil bath pan, control temperature for 80 DEG C, phosphorus source/arsenic source mixed solution is controlled into speed by peristaltic pump
5mL/min is added drop-wise to Ca (NO3)2·4H2In O (analysis is pure) solution, the amount of dropwise addition meets mol ratio Ca/ (P+As)=1.67;Drop
Add after finishing, the sustained response 5h at 60 DEG C, after reaction is aged 48h at room temperature after terminating, centrifuge washing, then at 55 DEG C
20h is dried, is ground after drying, obtain mixing arsenic hydroxyapatite presoma powder;
(3) the arsenic hydroxyapatite presoma powder of mixing that will be obtained is placed in Muffle furnace, is heated up with 5 DEG C/min heating rates
To 700 DEG C of insulation 3h, then room temperature is cooled to 5 DEG C/min rate of temperature fall, obtains mixing arsenic hydroxyapatite/calcium phosphate powder.
The arsenic doping amount and sintering temperature of mixing arsenic hydroxyapatite/calcium phosphate powder sample of obtained different arsenic doping amounts
As shown in table 2.
Table 2 respectively mixes the arsenic doping amount and sintering temperature of arsenic hydroxyapatite/calcium phosphate powder
Sample | Mix arsenic amount (wt%) | Sintering temperature (DEG C) |
11 | 0 | 700 |
12 | 0.5 | 700 |
13 | 3 | 700 |
14 | 5 | 700 |
15 | 10 | 700 |
The XRD for mixing arsenic hydroxyapatite/calcium phosphate powder sample of different arsenic doping amounts is as shown in figure 4, can by Fig. 4
Know after 700 DEG C of heat treatments, when arsenic doping amount is smaller (≤3wt.%), occur without new peak, illustrate that HA is undecomposed;Work as arsenic doping
When measuring larger (>=5.0wt.%), there is new diffraction maximum to occur, new peak is corresponding with the peak of β-TCP, illustrates to generate β-TCP.
Embodiment 3
900 DEG C of sintering prepare arsenic doping amount and mix arsenic hydroxyl phosphorus for 0wt%, 0.5wt%, 3wt%, 5wt% and 10wt%
Lime stone/calcium phosphate powder.
(1) by 0.1mol/L Na3AsO4(analysis is pure) solution and 0.25mol/L (NH4)3PO4·3H2O (analysis is pure) solution
Mixing and stirring, obtains phosphorus source/arsenic source mixed solution, and adjust mixed solution pH=10 with concentrated ammonia liquor;In 0.5mol/L Ca
(NO3)2·4H2The polyethylene glycol dispersant that 0.3wt% molecular weight is 6000,30min points of stirring are added in O (analysis is pure) solution
After dissipating uniformly, pH=11 is adjusted with concentrated ammonia liquor;
(2) in oil bath pan, control temperature for 80 DEG C, phosphorus source/arsenic source mixed solution is controlled into speed by peristaltic pump
3mL/min is added drop-wise to Ca (NO3)2·4H2In O (analysis is pure) solution, the amount of dropwise addition meets mol ratio Ca/ (P+As)=1.67;Drop
Add after finishing, the sustained response 4h at 70 DEG C, after reaction is aged 30h at room temperature after terminating, centrifuge washing, then at 50 DEG C
24h is dried, is ground after drying, obtain mixing arsenic hydroxyapatite presoma powder;
(3) the arsenic hydroxyapatite presoma powder of mixing that will be obtained is placed in Muffle furnace, is heated up with 5 DEG C/min heating rates
To 900 DEG C of insulation 3h, then room temperature is cooled to 5 DEG C/min rate of temperature fall, obtains mixing arsenic hydroxyapatite/calcium phosphate powder.
The arsenic doping amount and sintering temperature of mixing arsenic hydroxyapatite/calcium phosphate powder sample of obtained different arsenic doping amounts
As shown in table 3.
Table 3 respectively mixes the arsenic doping amount and sintering temperature of arsenic hydroxyapatite/calcium phosphate powder
Sample | Mix arsenic amount (wt%) | Sintering temperature (DEG C) |
21 | 0 | 900 |
22 | 0.5 | 900 |
23 | 3 | 900 |
24 | 5 | 900 |
25 | 10 | 900 |
The XRD for mixing arsenic hydroxyapatite/calcium phosphate powder sample of different arsenic doping amounts is as shown in figure 5, can by Fig. 5
Know, after 900 DEG C of heat treatments, the XRD diffraction peak intensities enhancing of all samples;And when arsenic doping amount is smaller (≤1wt%), without new
Peak occurs, and illustrates that HA is undecomposed;When arsenic doping amount is larger (>=3.0wt%), there are new diffraction maximum appearance, new peak and β-TCP
Peak it is corresponding, illustrate to generate β-TCP.Meanwhile, with the increase of arsenic doping amount, β-TCP mutually increase, and arsenic doping amount is increased to
During 10wt%, HA phases are completely converted into β-TCP phases.
Embodiment 4
1100 DEG C of sintering prepare arsenic doping amount and mix arsenic hydroxyl phosphorus for 0wt%, 0.5wt%, 3wt%, 5wt% and 10wt%
Lime stone/calcium phosphate powder.
(1) by 0.1mol/L Na3AsO4(analysis is pure) solution and 0.25mol/L (NH4)3PO4·3H2O (analysis is pure) solution
Mixing and stirring, obtains phosphorus source/arsenic source mixed solution, and adjust mixed solution pH=10 with concentrated ammonia liquor;In 0.5mol/L Ca
(NO3)2·4H2The polyethylene glycol dispersant that 0.3wt% molecular weight is 6000,30min points of stirring are added in O (analysis is pure) solution
After dissipating uniformly, pH=11 is adjusted with concentrated ammonia liquor;
(2) in oil bath pan, control temperature for 80 DEG C, phosphorus source/arsenic source mixed solution is controlled into speed by peristaltic pump
4mL/min is added drop-wise to Ca (NO3)2·4H2In O (analysis is pure) solution, the amount of dropwise addition meets mol ratio Ca/ (P+As)=1.67;Drop
Add after finishing, the sustained response 3h at 80 DEG C, after reaction is aged 24h at room temperature after terminating, centrifuge washing, then at 60 DEG C
12h is dried, is ground after drying, obtain mixing arsenic hydroxyapatite presoma powder;
(3) the arsenic hydroxyapatite presoma powder of mixing that will be obtained is placed in Muffle furnace, is heated up with 5 DEG C/min heating rates
To 1100 DEG C of insulation 3h, then room temperature is cooled to 5 DEG C/min rate of temperature fall, obtains mixing arsenic hydroxyapatite/calcium phosphate powder.
The arsenic doping amount and sintering temperature of mixing arsenic hydroxyapatite/calcium phosphate powder sample of obtained different arsenic doping amounts
As shown in table 4.
Table 4 respectively mixes the arsenic doping amount and sintering temperature of arsenic hydroxyapatite/calcium phosphate powder
Sample | Mix arsenic amount (wt%) | Sintering temperature (DEG C) |
31 | 0 | 1100 |
32 | 0.5 | 1100 |
33 | 3 | 1100 |
34 | 5 | 1100 |
35 | 10 | 1100 |
The XRD for mixing arsenic hydroxyapatite/calcium phosphate powder sample of different arsenic doping amounts is as shown in fig. 6, can by Fig. 6
Know, after 1100 DEG C of heat treatments, the XRD diffraction peak intensities enhancing of all samples;When arsenic doping amount is 1wt%, appearance is begun to
β-TCP phases;Meanwhile, with the increase of arsenic incorporation, HA is more easily decomposed into β-TCP phases, when arsenic doping amount increases to 10wt%, HA
Mutually it is completely converted into β-TCP phases.
The FTIR for mixing arsenic hydroxyapatite/calcium phosphate powder sample of different arsenic doping amounts is schemed as shown in fig. 7, can by Fig. 7
Know, with increasing for arsenic incorporation, OH-Absorption peak strength reduction, until disappear, carbonate HA it is intracell replacement with B
Type is changed into based on A types.Thus infer that arsenic mixes the site of part phosphate radical, the site that carbonate occupies phosphate radical then subtracts
It is few, 943cm in figure-1And 550cm-1Place have also appeared the characteristic peak of β-TCP, it was confirmed that the presence of β-TCP phases.
To sum up, the present invention is prepared and mixes arsenic hydroxyapatite/calcium phosphate powder, because the incorporation of arsenic easily makes hydroxyapatite whisker
Lattice internal structure produces defect, so as to be also easy to produce phase change in sintering process, makes HA inversion of phases be β-TCP phases.Preparation process
In, the arsenic hydroxyapatite presoma powder of mixing by arsenic doping amount in 0.1~10wt% intervals is sintered at 700~1100 DEG C,
The biophasic calcium phosphate ceramic powder of different HA/ β-TCP ratios is obtained, doping is higher, and the content of β-TCP phases is higher.
Meanwhile, the ratio of HA/ β-TCP is further obtained, HA in the BCP of gained can be analyzed using XRD refine software
And the phase content of β-TCP, then the biphasic calcium phosphate material that specific required HA/ β-TCP ratios are obtained by regulating and controlling the incorporation of arsenic
Material.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by the embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. one kind mixes arsenic hydroxyapatite/calcium phosphate powder, it is characterised in that described to mix arsenic hydroxyapatite/calcium phosphate powder
Particle is rod-like structure long, and the length of rod-shaped particles long is 80~150nm, and the width of rod-shaped particles long is 20~50nm.
2. the one kind according to claim 1 mixes arsenic hydroxyapatite/calcium phosphate powder, it is characterised in that described to mix arsenic
In hydroxyapatite/calcium phosphate powder, arsenate instead of part phosphate radical, and the doping of arsenic is 0.1~10wt%, mol ratio
Ca:(P+As)=1.67.
3. the one kind described in claim 1 or 2 mixes arsenic hydroxyapatite/calcium phosphate raw powder's production technology, it is characterised in that bag
Include following steps:
(1) after by arsenic source solution and phosphorus source solution mixing and stirring, it is added drop-wise in calcium source solution;Continue after completion of dropping anti-
Should, reaction is aged after terminating, is centrifuged, dries, grinding, and obtains mixing arsenic hydroxyapatite presoma powder;
(2) arsenic hydroxyapatite presoma powder will be mixed it will be placed in Muffle furnace and sinter, cooling will obtain described mixing arsenic hydroxy-apatite
Stone/calcium phosphate powder.
4. one kind according to claim 3 mixes arsenic hydroxyapatite/calcium phosphate raw powder's production technology, it is characterised in that
In step (1), arsenic source solution is Na3AsO4Solution, concentration is 0.1mol/L;Phosphorus source solution is (NH4)3PO4·
3H2O solution, concentration is 0.25mol/L;The calcium source solution is Ca (NO3)2·4H2O solution, concentration is 0.5mol/L.
5. one kind according to claim 3 mixes arsenic hydroxyapatite/calcium phosphate raw powder's production technology, it is characterised in that
In step (1), arsenic source solution adjusts pH to more than or equal to 10 with the mixed mixed solution of phosphorus source solution with concentrated ammonia liquor;
The calcium source solution adjusts pH to being more than or equal to 11, and addition before the mixed solution in phosphorus source and arsenic source is added dropwise with concentrated ammonia liquor
Dispersant is disperseed, and the addition of dispersant is 0.3~0.4wt% of calcium source solution.
6. one kind according to claim 5 mixes arsenic hydroxyapatite/calcium phosphate raw powder's production technology, it is characterised in that
In step (1), the dispersant is polyethylene glycol, and the molecular weight of polyethylene glycol is 6000.
7. one kind according to claim 3 mixes arsenic hydroxyapatite/calcium phosphate raw powder's production technology, it is characterised in that
In step (1), using peristaltic pump control, the speed of dropwise addition is 3~5mL/min to the speed of the dropwise addition.
8. one kind according to claim 3 mixes arsenic hydroxyapatite/calcium phosphate raw powder's production technology, it is characterised in that
In step (1), the temperature of the reaction is 60~80 DEG C, and the time of reaction is 3~5h;The time of the ageing is 24~48h.
9. one kind according to claim 3 mixes arsenic hydroxyapatite/calcium phosphate raw powder's production technology, it is characterised in that
In step (1), the drying is in 50~60 DEG C of 12~24h of drying.
10. one kind according to claim 3 mixes arsenic hydroxyapatite/calcium phosphate raw powder's production technology, it is characterised in that
In step (2), the sintering is to be warming up to 700~1100 DEG C of insulation 3h with the heating rate of 5~10 DEG C/min;The cooling is
Normal temperature is down to the rate of temperature fall of 5~10 DEG C/min.
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