CN1194775C - Ti surface HA active coating biological material and its preparation method - Google Patents
Ti surface HA active coating biological material and its preparation method Download PDFInfo
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- CN1194775C CN1194775C CNB021309094A CN02130909A CN1194775C CN 1194775 C CN1194775 C CN 1194775C CN B021309094 A CNB021309094 A CN B021309094A CN 02130909 A CN02130909 A CN 02130909A CN 1194775 C CN1194775 C CN 1194775C
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- Prior art keywords
- coating
- biological material
- powder
- active coating
- sintering
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- 238000000576 coating method Methods 0.000 title claims abstract description 45
- 239000011248 coating agent Substances 0.000 title claims abstract description 44
- 239000012620 biological material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims description 9
- 239000000843 powder Substances 0.000 claims abstract description 21
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 15
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 5
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims description 17
- 238000009413 insulation Methods 0.000 claims description 8
- 239000011159 matrix material Substances 0.000 claims description 3
- 239000011247 coating layer Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 239000011812 mixed powder Substances 0.000 abstract description 3
- 238000002490 spark plasma sintering Methods 0.000 abstract 3
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000004663 powder metallurgy Methods 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 33
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 8
- 229910052719 titanium Inorganic materials 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000002161 passivation Methods 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000001652 electrophoretic deposition Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000004826 seaming Methods 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
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- Materials For Medical Uses (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to HA active coating biological material on a Ti surface and a preparing method thereof, which belongs to the technical field of powder metallurgy. The material is characterized in that A coating on the surface of Ti matrices comprises 80 to 96 wt% of hydroxyapatite (hereinafter abbreviated as HA), 0 to 14 wt% of Ti and 4 to 6 wt% of water glass. The preparing method comprises: HA powder and mixed powder of HA and Ti are adopted, and water glass as a passivating agent is added to form coating material on a Ti surface; the coating material is spread on a Ti surface in a mold and then is put into a spark plasma sintering device (SPS), the SPS is pumped into pump and is pressured to 20 to 30MPa, and the temperature is increased rapidly to 850 to 950 DEG C at the speed of 80 to 150 DEG C/min and is kept for 2 to 10 min. The HA active coating biological material on a Ti surface, which is prepared by the method, has high interfacial bond strength and realizes the metallurgical bonding between Ti and HA.
Description
Technical field
A kind of preparation method of Ti surface HA active coating biological material belongs to powder metallurgical technology.
Background technology
Titanium surface hydroxyl apatite (being designated hereinafter simply as HA) active coating material combines metal Ti favorable mechanical performance and HA excellent biological compatibility and biological activity, is the material of the biological hard tissue implantation body that is expected at present.A lot of in Ti surface-coated HA coating process at present, as plasma spraying, laser melting coating, collosol and gel, acid-alkali treatment and electrophoretic deposition etc., a subject matter of existence is that coating and high base strength are low, easily produces behind the implant into body and peels off.The present invention adopts discharge plasma sintering technique (SPS) preparation Ti surface HA active coating biological material, and this technology has characteristics such as sintering temperature is low, temperature retention time is short, sintering mechanism is special.The Ti surface HA active coating biological material that makes by this technology has the interface bond strength height, and HA does not decompose, and is characteristics such as metallurgical bonding interface between Ti and the HA.
Summary of the invention
Problem to be solved by this invention is to overcome the problem that exists in the said method, and a kind of interface bond strength height is provided, and realizes metallurgical binding between Ti and the HA, and the Ti surface has biomaterial of HA active coating and preparation method thereof.
Ti surface HA active coating biological material provided by the invention is characterized in that the coating of Ti matrix surface is the hydroxyapatite (being designated hereinafter simply as HA) of 80-96% by percentage by weight, the Ti of 0-14%, and 4～6% waterglass is formed.
The preparation method of Ti surface HA active coating provided by the present invention is characterized in that, it may further comprise the steps: (1) is mixed HA, Ti and waterglass and is obtained the coating powder, toast by above-mentioned percentage by weight, waterglass plays the effect of passivator; (2) the Ti above-mentioned coating powder 0.1～0.3g that packs on the surface in mould guarantees that coating layer thickness is 0.1～0.3mm behind the sintering; (3) put into discharge plasma sintering (SPS) equipment, be evacuated to 4～10Pa, pressurization 20～30 MPa are rapidly heated under 80～150 ℃/min to 850～950 ℃ and carry out sintering, insulation 2～10min, cooling.
The present invention has added a certain amount of waterglass as passivator on the prescription of material, improved the interface bond strength of coating and matrix, has reduced the space that venting causes in the sintering.The present invention has adopted the preparation method of discharge plasma sintering, under special sintering mechanism, has realized the low temperature Fast Sintering, guarantees that HA does not decompose, and has obtained the high Ti surface HA active coating of bond strength.
The bond strength of 5 embodiment has all reached European commercial standard (CS) (more than the bond strength 28MPa), and test result sees Table 1.The combination interface microstructure picture of embodiment 1 as shown in Figure 3, with combination interface microstructure picture (shown in Figure 2) contrast of the HA coating of Ti surface unpassivated as seen, add waterglass passivator after, the space disappearance, sintering is fine and close more, has realized metallurgical binding.
Description of drawings
Fig. 1: agglomerating mould sketch map.
The microphotograph of Fig. 2: Ti surface HA coating interface (not adding waterglass).
The microphotograph of Fig. 3: Ti surface HA coating interface (adding waterglass).
F is an applied pressure among Fig. 1; 1. mould seaming chuck, 2. carbon paper, 3. coating powder, 4.Ti powder, 5. die coat, 6. mould push-down head.
The specific embodiment
Embodiment 1. get HA4.8g and waterglass 0.1g put into mix powder machine mix homogeneously after, in 100 ℃ of bakings 1 hour down, the HA powder that obtains passivation is as the coating powder 1. in baking oven.Get titanium valve 5.0g respectively, coating powder 1. 0.1g is packed in the graphite jig of φ 24, load onto the pressure head compacting, put into discharging plasma sintering equipment (SPS) then, be evacuated to 4Pa, plus-pressure 30MPa, programming rate is 150 ℃/min, be warming up to 900 ℃ of insulation 2min, be cooled to room temperature and take out, obtain the Ti surface HA active coating biological material.
Embodiment 2. gets titanium valve 5.0g respectively, coating powder 1. 0.2g is packed in the graphite jig of φ 24, load onto the pressure head compacting, put into SPS then, be evacuated to 10Pa, plus-pressure 20MPa, programming rate is 80 ℃/min, be warming up to 850 ℃ of insulation 10min, be cooled to room temperature and take out, obtain the Ti surface HA active coating biological material.
Embodiment 3. get HA4.0g, titanium valve 0.7g and waterglass 0.3g put into mix powder machine mix homogeneously after, in baking oven,, obtain the HA mixed powder of passivation, 2. as the coating powder in 100 ℃ of bakings 1 hour down.Get titanium valve 5.0g respectively, coating powder 2. 0.1g is packed in the graphite jig of φ 24, load onto the pressure head compacting, put into SPS then, be evacuated to 6Pa, plus-pressure 25MPa, programming rate is 150 ℃/min, be warming up to 950 ℃ of insulation 6min, be cooled to room temperature and take out, obtain the Ti surface HA active coating biological material.
Embodiment 4. gets HA4.5g, and titanium valve 0.3g and waterglass 0.2g toasted 1 hour down in 100 ℃ in baking oven after putting into and mixing powder machine mix homogeneously, obtained the HA mixed powder of passivation, as the coating powder 3..Get titanium valve 5.0g respectively, coating powder 3. 0.2g is packed in the graphite jig of φ 24, load onto the pressure head compacting, put into SPS then, be evacuated to 4Pa, plus-pressure 30MPa, 150 ℃/min of programming rate is warming up to 900 ℃ of sintering, insulation 6min, be cooled to room temperature and take out, obtain the biomaterial of Ti surface HA active coating.
Embodiment 5. gets titanium valve 5.0g respectively, the coating powder 1. 0.1g and coating powder 2. 0.1g pack in the graphite jig of φ 24, load onto the pressure head compacting, put into SPS then, be evacuated to 4Pa, plus-pressure 30MPa, 100 ℃/min of programming rate, be warming up to 900 ℃ of insulation 3min, be cooled to room temperature and take out, obtain the Ti surface HA active coating biological material.
Table 1
| Tensile force (kN) | Bond strength (MPa) | |
| Embodiment 1 | 20.5 | 45 |
| Embodiment 2 | 15.1 | 33 |
| Embodiment 3 | 28.9 | 64 |
| Embodiment 4 | 17.4 | 38 |
| Embodiment 5 | 16.0 | 35 |
Claims (3)
1, a kind of Ti surface HA active coating biological material is characterized in that: the coating of Ti matrix surface is the hydroxyapatite of 80-96% by percentage by weight, the Ti of 0-14%, and 4～6% waterglass is formed.
2, a kind of preparation method of Ti surface HA active coating biological material, it is characterized in that, it may further comprise the steps: (1) is the hydroxyapatite of 80-96% with percentage by weight, the Ti of 0-14%, 4～6% waterglass mixes and obtains the coating powder, toast, waterglass plays the effect of passivator; (2) the Ti above-mentioned coating powder 0.1～0.3g that packs on the surface in mould guarantees that coating layer thickness is 0.1～0.3mm behind the sintering; (3) put into discharging plasma sintering equipment, be evacuated to 4～10Pa, pressurization 20～30MPa is rapidly heated under 80～150 ℃/min to 850～950 ℃ and carries out sintering, insulation 2～10min, cooling.
3, preparation method according to claim 2 is characterized in that, evacuation 4～5Pa in the step (3), pressurization 28～30MPa, 100～120 ℃/min of heating rate, 870～900 ℃ of sintering temperatures, insulation 3～5min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021309094A CN1194775C (en) | 2002-09-13 | 2002-09-13 | Ti surface HA active coating biological material and its preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021309094A CN1194775C (en) | 2002-09-13 | 2002-09-13 | Ti surface HA active coating biological material and its preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN1400022A CN1400022A (en) | 2003-03-05 |
| CN1194775C true CN1194775C (en) | 2005-03-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB021309094A Expired - Fee Related CN1194775C (en) | 2002-09-13 | 2002-09-13 | Ti surface HA active coating biological material and its preparation method |
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| CN (1) | CN1194775C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1302820C (en) * | 2005-09-16 | 2007-03-07 | 哈尔滨工程大学 | Bone tissue rack of TiO2 reinforced polyhydroxyethyl methacrylate and its prepn process |
| FR2892621B1 (en) * | 2005-10-27 | 2009-08-21 | Protip Sas Soc Par Actions Sim | PROCESS FOR OBTAINING A BIOCOMPATIBLE COMPOSITE IMPLANT |
| CN102631704A (en) * | 2012-04-20 | 2012-08-15 | 中原工学院 | Titanium-aluminium based hydroxyapatite coating and preparation method thereof |
| CN104841009B (en) * | 2015-04-21 | 2017-08-25 | 昆明理工大学 | A kind of hydroxyapatite activation titanium alloy top layer Biocomposite material and preparation method thereof |
| CN104857562B (en) * | 2015-04-21 | 2018-06-19 | 昆明理工大学 | A kind of titanium alloy/calcium pyrophosphate surface layer Biocomposite material and preparation method thereof |
| CN105458271B (en) * | 2016-01-12 | 2017-11-24 | 中南大学 | A kind of titanium alloy composite material coated with composite coating and its preparation method and application |
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2002
- 2002-09-13 CN CNB021309094A patent/CN1194775C/en not_active Expired - Fee Related
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| CN1400022A (en) | 2003-03-05 |
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