CN108118526B - Preparation method of super-large calcium hydrogen phosphate dihydrate with surface in flower cluster shape - Google Patents
Preparation method of super-large calcium hydrogen phosphate dihydrate with surface in flower cluster shape Download PDFInfo
- Publication number
- CN108118526B CN108118526B CN201711328466.4A CN201711328466A CN108118526B CN 108118526 B CN108118526 B CN 108118526B CN 201711328466 A CN201711328466 A CN 201711328466A CN 108118526 B CN108118526 B CN 108118526B
- Authority
- CN
- China
- Prior art keywords
- solution
- calcium
- carbon fiber
- sample
- dihydrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
- D06M11/71—Salts of phosphoric acids
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0607—Wires
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials For Medical Uses (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a preparation method of super-large calcium hydrogen phosphate dihydrate with a flower-like cluster surface, which takes carbon fiber as a base material, improves the surface structure of the carbon fiber through chemical vapor deposition treatment, provides a proper nucleation site for promoting the rapid generation of the calcium hydrogen phosphate dihydrate, and then adopts a pulse electrodeposition process to prepare the calcium hydrogen phosphate dihydrate. The maximum average growth rate of the calcium hydrophosphate dihydrate prepared by the method can reach 1290 mu m/h, which is 12.9 times of the maximum growth rate of the calcium hydrophosphate dihydrate reported in the background art. In addition, the surface of the calcium hydrophosphate dihydrate prepared by the method is in a flower cluster shape, and the flower cluster-shaped surface structure is favorable for the attachment of cells and the formation of bone tissues.
Description
Technical Field
The invention belongs to a preparation method of biological materials, and relates to a preparation method of super-large sheet calcium hydrogen phosphate dihydrate with a flower-like cluster surface.
Background
The calcium-phosphorus bioceramics mainly comprise hydroxyapatite (Ca)10(PO4)6(OH)2HA), dibasic calcium phosphate dihydrate (CaHPO)4·2H2O, DCPD), tricalcium phosphate (Ca)3(PO4)2TCP). Of these, calcium hydrogen phosphate dihydrate is widely used as a biomedical material because of its excellent biocompatibility and osteoconductive properties. It has similarity with the components and structure of human bone, low solubility in body fluid or blood plasma, no toxicity, harm and carcinogenesis, excellent bioactivity, osteoconductivity and biocompatibility, and may be used widely in repairing damaged bone tissue, repairing tooth root in alveolar ridge, repairing hip joint and knee joint, coating of bone tissue, etc. Therefore, many researchers have conducted research on the preparation of calcium hydrogen phosphate dihydrate.
In the literature 1, "Liu G Y, Tang S W, Wang C, et al, Formation characterization of Ca-Pcoatings on magnesium alloy surface, Chinese non-ferrous metals bulletin (English edition), 2013,23(8): 2294-.
Document 2 "ZHao C L, Wu H L, Hou P, et al, enhanced chromatography resistance and performance of Zn doped DCPD coating on biogradeable Mg. materials letters,2016,180: 42-46" reports that 1 hour is used to prepare a sheet-like calcium hydrogen phosphate dihydrate having a length of 50-100 μm, a maximum length of 100 μm, a smooth surface and a maximum average growth rate of 100 μm/H.
Document 3 "Zhang C Y, Zeng R C, Chen R S, et al.preparation of calcium phosphate coatings on Mg-1.0Ca alloy. Chinese non-ferrous metals bulletin (English edition), 2010,20(S2): S655-S659" reports that calcium hydrogen phosphate dihydrate having a length of 20 to 200 μm is prepared in 2 hours, the maximum length is 200 μm, the surface is smooth, and the maximum average growth rate is 100 μm/h.
The documents successfully prepare the calcium hydrophosphate dihydrate, but the maximum average growth speed of the prepared calcium hydrophosphate dihydrate is less than 100 mu m/h, and the growth speed is slow. And the surfaces of the prepared calcium hydrophosphate dihydrate are smooth, so that the cells are not favorably attached to the surfaces of the calcium hydrophosphate dihydrate and the formation of bone tissues is not favorably realized.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a preparation method of super-large calcium hydrogen phosphate dihydrate with a flower-shaped cluster surface, which takes carbon fibers as a base material, improves the surface structure of the carbon fibers through chemical vapor deposition treatment, provides a proper nucleation site for promoting the rapid generation of the calcium hydrogen phosphate dihydrate, and then adopts a pulse electrodeposition process to prepare the calcium hydrogen phosphate dihydrate. The maximum average growth rate of the calcium hydrophosphate dihydrate prepared by the method can reach 1290 mu m/h, which is 12.9 times of the maximum growth rate of the calcium hydrophosphate dihydrate reported in the background art.
Technical scheme
A preparation method of super large calcium hydrogen phosphate dihydrate with a flower-like cluster-shaped surface is characterized by comprising the following steps:
step 1: placing carbon fibers in a chemical vapor deposition furnace for deposition, wherein the parameters are as follows: heating to 1050-;
ultrasonically cleaning the deposited carbon fiber by acetone and then drying;
step 2: putting the carbon fiber deposited in the step (1) into a solution, taking a graphite sheet as an anode and the carbon fiber deposited as a cathode, applying a voltage of 3-5V between the two electrodes, wherein the deposition time is 15-25min and the deposition temperature is 40-60 ℃; the pulse width of the voltage is 50-100ms, and the pulse interval is 100-200 ms; the distance between the cathode and the anode is 30-50 mm;
the solution is as follows: dissolving ammonium dihydrogen phosphate in deionized water to prepare a solution of 60-150mmol/L, adding calcium nitrate, and uniformly stirring to obtain a solution; the molar ratio of the calcium nitrate to the ammonium dihydrogen phosphate is 1.7-2.0;
and step 3: placing the carbon fiber treated in the step 2 in a metal spraying instrument under the pressure of 4 multiplied by 10-2-6×10-2Spraying gold for 60-100s under the condition of Pa and current of 6-8 mA;
and 4, step 4: placing a sample C in the solution, setting the applied voltage to be 1-3V by taking a graphite sheet as an anode and a sample C as a cathode, setting the deposition time to be 5-10min and the deposition temperature to be 60-70 ℃, taking out the sample after the reaction is finished, and drying the sample to obtain the super-large sheet calcium hydrophosphate dihydrate with the surface in the shape of a flower cluster;
the pulse width of the voltage is 20-40ms, and the pulse interval is 50-100 ms;
the distance between the cathode and the anode is 30-50 mm;
the solution is as follows: dissolving ammonium dihydrogen phosphate in deionized water to prepare a solution of 10-30mmol/L, adding calcium nitrate, and uniformly stirring to obtain a solution; the molar ratio of the calcium nitrate to the ammonium dihydrogen phosphate is 1.0-1.5.
The ultrasonic cleaning is carried out for 5-10min by adopting acetone.
Advantageous effects
The invention provides a preparation method of super-large calcium hydrogen phosphate dihydrate with a flower-like cluster surface, which takes carbon fiber as a base material, improves the surface structure of the carbon fiber through chemical vapor deposition treatment, provides a proper nucleation site for promoting the rapid generation of the calcium hydrogen phosphate dihydrate, and then adopts a pulse electrodeposition process to prepare the calcium hydrogen phosphate dihydrate. The maximum average growth rate of the calcium hydrophosphate dihydrate prepared by the method can reach 1290 mu m/h, which is 12.9 times of the maximum growth rate of the calcium hydrophosphate dihydrate reported in the background art. In addition, the surface of the calcium hydrophosphate dihydrate prepared by the method is in a flower cluster shape, and the flower cluster-shaped surface structure is favorable for the attachment of cells and the formation of bone tissues.
Drawings
FIG. 1 is a scanning electron micrograph of dibasic calcium phosphate dihydrate prepared in example 2
FIG. 2 is an X-ray diffraction pattern of dibasic calcium phosphate dihydrate prepared in example 2
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1:
(1) placing the carbon fiber in a chemical vapor deposition furnace, heating to 1050 ℃ at the speed of 8 ℃/min, then introducing methane with the flow rate of 0.4L/min, argon with the flow rate of 0.1L/min and hydrogen with the flow rate of 0.3L/min, and depositing for 1.5 h. Ultrasonically cleaning the deposited sample for 5min by acetone in sequence, and marking the dried sample as A;
(2) dissolving ammonium dihydrogen phosphate in deionized water to prepare a solution of 60mmol/L, preparing a calcium nitrate solution according to the molar ratio of calcium nitrate to ammonium dihydrogen phosphate of 1.7, and uniformly mixing the calcium nitrate and the ammonium dihydrogen phosphate to obtain a solution I. Dissolving ammonium dihydrogen phosphate in deionized water to prepare a solution of 10mmol/L, preparing a calcium nitrate solution according to the molar ratio of calcium nitrate to ammonium dihydrogen phosphate of 1.0, and uniformly mixing the calcium nitrate and the ammonium dihydrogen phosphate to obtain a solution II;
(3) placing a sample A in the solution I, taking a graphite sheet as an anode and a sample A as a cathode, wherein the distance between the cathode and the anode is 30mm, applying a voltage of 3V, the pulse width is 50ms, the pulse interval is 100ms, the deposition time is 15min, the deposition temperature is 40 ℃, and the sample obtained after the reaction is finished is marked as B;
(4) sample B was placed in a metal spraying apparatus at a pressure of 4X 10-2Spraying gold for 60s under the condition of Pa and 6mA of current, and marking an obtained sample as C;
(5) sample C was placed in solution II with graphite sheet as the anode and sample C as the cathode, the distance between the cathode and the anode was 30mm, the applied voltage was set to 1V, the pulse width was 20ms, the pulse interval was 50ms, the deposition time was 5min, and the deposition temperature was 60 ℃. And after the reaction is finished, taking out the sample and drying to obtain the surface flower-like ultra-large calcium hydrophosphate dihydrate.
The average growth rate of dibasic calcium phosphate dihydrate prepared in this example 1 was 620 μm/h.
Example 2:
(1) placing the carbon fiber in a chemical vapor deposition furnace, heating to 1100 ℃ at the speed of 10 ℃/min, then introducing methane with the flow rate of 0.5L/min, argon with the flow rate of 0.2L/min and hydrogen with the flow rate of 0.5L/min, and depositing for 2.0 h. Ultrasonically cleaning the deposited sample for 10min by acetone in sequence, and marking the dried sample as A;
(2) ammonium dihydrogen phosphate was dissolved in deionized water to prepare a 100mmol/L solution, a calcium nitrate solution was prepared at a molar ratio of calcium nitrate to ammonium dihydrogen phosphate of 1.7, and the calcium nitrate and ammonium dihydrogen phosphate were mixed uniformly and recorded as solution I. Dissolving ammonium dihydrogen phosphate in deionized water to prepare a solution with the concentration of 20mmol/L, preparing a calcium nitrate solution according to the molar ratio of 1.0 of calcium nitrate to ammonium dihydrogen phosphate, and uniformly mixing the calcium nitrate and the ammonium dihydrogen phosphate to obtain a solution II;
(3) placing a sample A in the solution I, taking a graphite sheet as an anode and a sample A as a cathode, wherein the distance between the cathode and the anode is 50mm, applying a voltage of 4V, the pulse width is 80ms, the pulse interval is 100ms, the deposition time is 20min, the deposition temperature is 50 ℃, and the sample obtained after the reaction is finished is marked as B;
(4) sample B was placed in a metal spraying apparatus at a pressure of 6X 10-2Spraying gold for 80s under the condition that the current is 8mA, and marking an obtained sample as C;
(5) sample C was placed in solution II with graphite sheet as the anode and sample C as the cathode, the distance between the cathode and the anode was 30mm, the applied voltage was set at 2V, the pulse width was 30ms, the pulse interval was 80ms, the deposition time was 8min, and the deposition temperature was 60 ℃. And after the reaction is finished, taking out the sample and drying to obtain the surface flower-like ultra-large calcium hydrophosphate dihydrate.
FIG. 1 is a scanning electron micrograph of dibasic calcium phosphate dihydrate prepared in example 2, from FIG. 1, it can be seen that the surface of a large piece of dibasic calcium phosphate dihydrate appears in a flower cluster shape. Fig. 2 is an X-ray diffraction pattern of dibasic calcium phosphate dihydrate prepared in example 2, and from fig. 2, it can be seen that the phase component of the prepared material was dibasic calcium phosphate dihydrate, without other impurities.
The average growth rate of dibasic calcium phosphate dihydrate prepared in this example 2 was 1290. mu.m/h.
Example 3:
(1) placing the carbon fiber in a chemical vapor deposition furnace, heating to 1050 ℃ at the speed of 10 ℃/min, then introducing methane with the flow rate of 0.6L/min, argon with the flow rate of 0.2L/min and hydrogen with the flow rate of 0.6L/min, and depositing for 2.5 h. Ultrasonically cleaning the deposited sample for 10min by acetone in sequence, and marking the dried sample as A;
(2) ammonium dihydrogen phosphate is dissolved in deionized water to prepare 150mmol/L solution, calcium nitrate solution is prepared according to the molar ratio of calcium nitrate to ammonium dihydrogen phosphate of 2.0, and the calcium nitrate and the ammonium dihydrogen phosphate are uniformly mixed and recorded as solution I. Dissolving ammonium dihydrogen phosphate in deionized water to prepare a solution with the concentration of 30mmol/L, preparing a calcium nitrate solution according to the molar ratio of 1.5 of calcium nitrate to ammonium dihydrogen phosphate, and uniformly mixing the calcium nitrate and the ammonium dihydrogen phosphate to obtain a solution II;
(3) placing a sample A in the solution I, taking a graphite sheet as an anode and a sample A as a cathode, wherein the distance between the cathode and the anode is 50mm, applying a voltage of 5V, the pulse width is 100ms, the pulse interval is 200ms, the deposition time is 25min, the deposition temperature is 60 ℃, and the sample obtained after the reaction is finished is marked as B;
(4) sample B was placed in a metal spraying apparatus at a pressure of 6X 10-2Spraying gold for 100s under the condition that the current is 8mA, and marking an obtained sample as C;
(5) sample C was placed in solution II with graphite sheet as the anode and sample C as the cathode, the distance between the cathode and the anode was 50mm, the applied voltage was set to 3V, the pulse width was 40ms, the pulse interval was 100ms, the deposition time was 10min, and the deposition temperature was 70 ℃. And after the reaction is finished, taking out the sample and drying to obtain the surface flower-like ultra-large calcium hydrophosphate dihydrate.
The average growth rate of dibasic calcium phosphate dihydrate prepared in this example 3 was 1010 μm/h.
Example 4:
(1) placing the carbon fiber in a chemical vapor deposition furnace, heating to 1200 ℃ at the speed of 8 ℃/min, then introducing methane with the flow rate of 0.4L/min, argon with the flow rate of 0.2L/min and hydrogen with the flow rate of 0.3L/min, and depositing for 1.5 h. Ultrasonically cleaning the deposited sample for 10min by acetone in sequence, and marking the dried sample as A;
(2) dissolving ammonium dihydrogen phosphate in deionized water to prepare a solution of 60mmol/L, preparing a calcium nitrate solution according to the molar ratio of calcium nitrate to ammonium dihydrogen phosphate of 2.0, and uniformly mixing the calcium nitrate and the ammonium dihydrogen phosphate to obtain a solution I. Dissolving ammonium dihydrogen phosphate in deionized water to prepare a solution of 10mmol/L, preparing a calcium nitrate solution according to the molar ratio of calcium nitrate to ammonium dihydrogen phosphate of 1.5, and uniformly mixing the calcium nitrate and the ammonium dihydrogen phosphate to obtain a solution II;
(3) placing a sample A in the solution I, taking a graphite sheet as an anode and a sample A as a cathode, wherein the distance between the cathode and the anode is 30mm, applying a voltage of 5V, the pulse width is 50ms, the pulse interval is 200ms, the deposition time is 15min, the deposition temperature is 60 ℃, and the sample obtained after the reaction is finished is marked as B;
(4) sample B was placed in a metal spraying apparatus at a pressure of 4X 10-2Spraying gold for 60s under the condition of Pa and current of 8mA, and marking an obtained sample as C;
(5) sample C was placed in solution II with graphite sheet as the anode and sample C as the cathode, the distance between the cathode and the anode was 50mm, the applied voltage was set at 1V, the pulse width was 40ms, the pulse interval was 50ms, the deposition time was 10min, and the deposition temperature was 60 ℃. And after the reaction is finished, taking out the sample and drying to obtain the surface flower-like ultra-large calcium hydrophosphate dihydrate.
The average growth rate of dibasic calcium phosphate dihydrate prepared in this example 4 was 930 μm/h.
Example 5:
(1) placing the carbon fiber in a chemical vapor deposition furnace, heating to 1000 ℃ at the speed of 10 ℃/min, then introducing methane with the flow rate of 0.5L/min, argon with the flow rate of 0.1L/min and hydrogen with the flow rate of 0.5L/min, and depositing for 2.0 h. Ultrasonically cleaning the deposited sample for 5min by acetone in sequence, and marking the dried sample as A;
(2) dissolving ammonium dihydrogen phosphate in deionized water to prepare a solution of 80mmol/L, preparing a calcium nitrate solution according to the molar ratio of calcium nitrate to ammonium dihydrogen phosphate of 2.0, and uniformly mixing the calcium nitrate and the ammonium dihydrogen phosphate to obtain a solution I. Dissolving ammonium dihydrogen phosphate in deionized water to prepare a solution with the concentration of 20mmol/L, preparing a calcium nitrate solution according to the molar ratio of 1.5 of calcium nitrate to ammonium dihydrogen phosphate, and uniformly mixing the calcium nitrate and the ammonium dihydrogen phosphate to obtain a solution II;
(3) placing a sample A in the solution I, taking a graphite sheet as an anode and a sample A as a cathode, wherein the distance between the cathode and the anode is 40mm, applying a voltage of 4V, the pulse width is 80ms, the pulse interval is 100ms, the deposition time is 20min, the deposition temperature is 50 ℃, and the sample obtained after the reaction is finished is marked as B;
(4) sample B was placed in a metal spraying apparatus at a pressure of 5X 10-2Spraying gold for 100s under the condition that the current is 6mA, and marking an obtained sample as C;
(5) sample C was placed in solution II with graphite sheet as the anode and sample C as the cathode, the distance between the cathode and the anode was 50mm, the applied voltage was set at 2V, the pulse width was 30ms, the pulse interval was 100ms, the deposition time was 10min, and the deposition temperature was 70 ℃. And after the reaction is finished, taking out the sample and drying to obtain the surface flower-like ultra-large calcium hydrophosphate dihydrate.
The average growth rate of dibasic calcium phosphate dihydrate prepared in this example 5 was 850. mu.m/h.
Claims (2)
1. A preparation method of super large calcium hydrogen phosphate dihydrate with a flower-like cluster-shaped surface is characterized by comprising the following steps:
step 1: placing carbon fibers in a chemical vapor deposition furnace for deposition, wherein the parameters are as follows: heating to 1050-;
ultrasonically cleaning the deposited carbon fiber by acetone and then drying;
step 2: putting the carbon fiber deposited in the step (1) into a solution, taking a graphite sheet as an anode and the carbon fiber deposited as a cathode, applying a voltage of 3-5V between the two electrodes, wherein the deposition time is 15-25min and the deposition temperature is 40-60 ℃; the pulse width of the voltage is 50-100ms, and the pulse interval is 100-200 ms; the distance between the cathode and the anode is 30-50 mm;
the solution is as follows: dissolving ammonium dihydrogen phosphate in deionized water to prepare a solution of 60-150mmol/L, adding calcium nitrate, and uniformly stirring to obtain a solution; the molar ratio of the calcium nitrate to the ammonium dihydrogen phosphate is 1.7-2.0;
and step 3: placing the carbon fiber treated in the step 2 in a metal spraying instrument under the pressure of 4 multiplied by 10-2-6×10-2Spraying gold for 60-100s under the condition of Pa and current of 6-8 mA;
and 4, step 4: placing the carbon fiber subjected to metal spraying in the step 3 into a solution, setting the applied voltage to be 1-3V by taking a graphite sheet as an anode and the carbon fiber subjected to metal spraying as a cathode, setting the deposition time to be 5-10min and the deposition temperature to be 60-70 ℃, taking out a sample after the reaction is finished, and drying the sample to obtain the ultra-large sheet calcium hydrophosphate dihydrate with the surface in a flower cluster shape;
the pulse width of the voltage is 20-40ms, and the pulse interval is 50-100 ms;
the distance between the cathode and the anode is 30-50 mm;
the solution is as follows: dissolving ammonium dihydrogen phosphate in deionized water to prepare a solution of 10-30mmol/L, adding calcium nitrate, and uniformly stirring to obtain a solution; the molar ratio of the calcium nitrate to the ammonium dihydrogen phosphate is 1.0-1.5.
2. The method for preparing super large calcium hydrogen phosphate dihydrate with surface clusters as claimed in claim 1, characterized in that: the ultrasonic cleaning is carried out for 5-10min by adopting acetone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711328466.4A CN108118526B (en) | 2017-12-13 | 2017-12-13 | Preparation method of super-large calcium hydrogen phosphate dihydrate with surface in flower cluster shape |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711328466.4A CN108118526B (en) | 2017-12-13 | 2017-12-13 | Preparation method of super-large calcium hydrogen phosphate dihydrate with surface in flower cluster shape |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108118526A CN108118526A (en) | 2018-06-05 |
| CN108118526B true CN108118526B (en) | 2020-05-01 |
Family
ID=62229090
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711328466.4A Active CN108118526B (en) | 2017-12-13 | 2017-12-13 | Preparation method of super-large calcium hydrogen phosphate dihydrate with surface in flower cluster shape |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108118526B (en) |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10369253B2 (en) * | 2011-10-31 | 2019-08-06 | The University Of Toledo | Method for modifying surfaces for better osseointegration |
| CN102552978A (en) * | 2012-02-20 | 2012-07-11 | 西北工业大学 | Method for preparing hydroxyapatite bioactive coating |
| CN103147280B (en) * | 2013-02-06 | 2014-07-16 | 西北工业大学 | Biological activity modified method of carbon fiber surface |
-
2017
- 2017-12-13 CN CN201711328466.4A patent/CN108118526B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN108118526A (en) | 2018-06-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101709496B (en) | Micro-arc oxidation-electrodeposition preparation method of magnesium-based bioactive coating | |
| Gopi et al. | A comparative study on the direct and pulsed current electrodeposition of hydroxyapatite coatings on surgical grade stainless steel | |
| CN101643929B (en) | Pulse electrodeposition preparation method of hydroxyapatite coating on surface of pure magnesium or magnesium alloy | |
| Chakraborty et al. | Synthesis of calcium hydrogen phosphate and hydroxyapatite coating on SS316 substrate through pulsed electrodeposition | |
| CN101249279B (en) | Method for using laser quick forming for producing HA/Ti gradient biological activity material | |
| Wijesinghe et al. | Preparation of bone-implants by coating hydroxyapatite nanoparticles on self-formed titanium dioxide thin-layers on titanium metal surfaces | |
| CN103272269B (en) | Hydroxyapatite/chitosan composite coating and preparation method thereof | |
| CN106676604B (en) | Preparation method and applications with the porous titanium of lattice structure or the antibacterial bioactive ceramics film of titanium alloy surface | |
| CN102090982B (en) | Artificial tooth root or joint material and microarc oxidation preparation method thereof | |
| US10369253B2 (en) | Method for modifying surfaces for better osseointegration | |
| CN101381881A (en) | Method for preparing hydroxylapatite/chitosan composite coating by pulse electrochemical deposition | |
| CN101254314A (en) | Hydroxylapatite coating magnesium alloy medical inner implantation material and method of preparing the same | |
| CN106267342A (en) | A kind of dentistry implant and preparation method thereof | |
| CN104436301A (en) | Preparation method of phytic acid/hydroxyapatite hybrid coating on magnesium alloy | |
| CN110042392A (en) | Preparation method of composite coating with excellent biocompatibility and antibacterial property on surface of medical implant | |
| Liu et al. | In simulated body fluid performance of polymorphic apatite coatings synthesized by pulsed electrodeposition | |
| CN107761148A (en) | A kind of method that fibroin albumen hydroxyapatite coating layer is prepared in metal surface | |
| CN108118526B (en) | Preparation method of super-large calcium hydrogen phosphate dihydrate with surface in flower cluster shape | |
| CN114681615A (en) | Preparation method and application of one-step synthesized Fe-doped hydroxyapatite | |
| WO2008146113A2 (en) | Process for coating a surface of a metal element to increase osteointegration thereof and prosthetic device including said element | |
| CN106283154B (en) | A kind of two step prepares method and the application of Mg alloy surface silico-calcium phosphorus bio-ceramic coating | |
| CN103184497A (en) | Electrochemical method for preparing fluorine-containing hydroxyapatite/zirconia transition coating on surface of medical titanium | |
| CN101161295A (en) | Method for modifying medical metallic grafting body surface collagen by galvano-chemistry method | |
| CN109179355B (en) | Metal oxide/calcium-phosphorus double-layer micron tube and preparation method thereof | |
| CN111363995B (en) | Preparation method of medical metal bone implant material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |