CN106334214B - A kind of multiple liquid phase construction method towards the preparation of calcium phosphate active ceramic bone bracket - Google Patents
A kind of multiple liquid phase construction method towards the preparation of calcium phosphate active ceramic bone bracket Download PDFInfo
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- CN106334214B CN106334214B CN201510408375.6A CN201510408375A CN106334214B CN 106334214 B CN106334214 B CN 106334214B CN 201510408375 A CN201510408375 A CN 201510408375A CN 106334214 B CN106334214 B CN 106334214B
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Abstract
The present invention discloses a kind of using K2CO3、Na2CO3And Li2CO3The formula that three kinds of materials are constituted forms multiple liquid phase, solves the preparation method for the problems such as sintering of calcium phosphate active ceramic is difficult, consistency is low when selective laser sintering, steps are as follows: by K2CO3、Na2CO3And Li2CO3In mass ratio 3: 2: 1 be uniformly mixed carbonate powder is prepared；94%~99% calcium phosphate active ceramic powder and 1%~6% carbonate powder are weighed in mass ratio, are uniformly mixed in alcohol by magnetic stirring apparatus；Powder after stirring is by obtaining composite powder after vacuum drying and ball milling；Composite powder is prepared into bone bracket by selective laser sintering.Preparation method of the present invention is easy, material source is extensive, and prepared compound rest has good mechanical property and biology performance.
Description
Technical field
K is utilized the present invention relates to a kind of2CO3、Na2CO3And Li2CO3The formula that three kinds of materials are constituted forms multiple liquid phase, solves
The problems such as certainly sintering of calcium phosphate active ceramic is difficult when selective laser sintering, consistency is low, while being generated using their decomposition
The method that gas forms microcellular structure necessary to bone bracket, belongs to bone tissue engineer field.
Background technique
Tissue engineered bone bracket should have good biocompatibility first to guarantee the safety of body, and certain mechanics is strong
Degree provides structural support for defect, and suitable microcellular structure grows, breaks up and is proliferated to be conducive to cell.Calcium phosphate activity
Ceramic mainly includes hydroxyapatite and tricalcium phosphate, is the important inorganic substances for constituting human body hard tissue, is implanted into after human body it
Surface can reach completely affine with tissue by the combination of chemical bond, therefore have good biocompatibility and biology
Activity, it is considered to be the alternative materials of most promising artificial bone.
However the associative key of calcium phosphate active ceramic is mainly ionic bond and covalent bond, the attraction of intermolecular particle is very
By force, lattice energy is big, thus self-diffusion coefficient is very low, keeps its sintering very difficult, it is also difficult to densify.Determine that it must be in height
Sintering temperature and long sintering time under could obtain the material of high-compactness, and the selective laser sintering time is very short, only
The sintering character of material is improved using the method for addition sintering aid so that sintering can not be carried out for Millisecond or Microsecond grade,
It is allowed to obtain fine and close material in a relatively short period of time as a kind of inevitable choice.
Introducing liquid phase is to improve material sintering character, improves mass transfer rate, realizes the effective ways of quick densifying.Because
Liquid phase can produce biggish capillary force, and under the action of capillary force, flowing and filling pore space occur for liquid phase；Meanwhile
Capillary force action but also solid particle force unbalance and generate grain slide, reset particle further.Sintering is completed
Afterwards, between liquid phase material is to fill and mutually there is solid particle, solid particle is connected, improves the consistency of calcium phosphate active ceramic, into
And improve its mechanical property.
This patent is quasi- to utilize potassium carbonate (K2CO3) melted at 891 DEG C, with sodium carbonate (Na2CO3) constitute binary composition exist
695 DEG C of congruent meltings, they and lithium carbonate (Li2CO3) ternary component that constitutes 399 DEG C of congruent meltings the characteristics of, construct it is a kind of 399 DEG C,
Triple liquid phases of 695 DEG C and 891 DEG C temperature spots offer liquid phases, to promote the sintering character of calcium phosphate active ceramic, and this
It can decompose in three kinds of carbonate sintering processes and generate gas, form microporous structure necessary to artificial bone scaffold, added
The lithium added can also promote symphysis, and sodium and potassium are all human body institute indispensable elements, further increase the biology of bone bracket
Energy.
Summary of the invention
The present invention utilizes K2CO3、Na2CO3、Li2CO3Three kinds of materials construct one kind in 399 DEG C, 695 DEG C and 891 DEG C temperature spots
The component of liquid phase is provided, solve in laser sintered calcium phosphate active ceramic bone stent procedures that material sintering is difficult, consistency is low and
The disadvantages of mechanical strength is insufficient, and microcellular structure needed for obtaining bone bracket using their pyrolytic characteristic.
The preparation method of calcium phosphate active ceramic bone bracket of the invention is implemented as follows:
One, potassium carbonate, sodium carbonate and lithium carbonate are mixed to get carbonate powder by certain mass weighing.According still further to certain matter
Amount percentage weighs calcium phosphate active ceramic powder and carbonate powder respectively, then by weighed powder difference in mass ratio 1:
9 are put into and are configured to 10% mixed liquor in alcohol and obtain uniformly mixed mixed liquor by magnetic stirrer；
Two, mixed liquor is filtered, is subsequently placed in vacuum oven, dry 6~8 is small under the conditions of 60 DEG C~80 DEG C
When, the mixed-powder after drying passes through ball milling 20~30 hours again, obtains the uniformly mixed composite powder of solid-state；
Three, composite powder that will be uniformly mixed is packed into the auxiliary powder system of selective laser, under nitrogen atmosphere, use diameter for
The laser facula of 0.8~1mm, the laser power of 6~7W, the sintering parameters such as scanning speed of 100~150mm/min are sintered
Preparation.
The mass ratio of potassium carbonate, sodium carbonate and lithium carbonate is 3: 2: 1 in the carbonate powder.
The mass percent of the calcium phosphate active ceramic powder and carbonate powder is respectively 94%~99% and 1%
~6%.
The magnetic agitation rotating speed is 1500r/min, and the time is 2-3 hours.
Advantage of the present invention is as follows:
(1) liquid phase is provided using potassium carbonate, sodium carbonate, lithium carbonate, overcomes calcium phosphate active ceramic sintering hardly possible, consistency
Low disadvantage, improves mechanical property.
(2) decomposition for utilizing potassium carbonate, sodium carbonate, lithium carbonate, obtains microcellular structure necessary to bone bracket, improves life
Object performance.
(3) lithium ion provided using lithium carbonate improves the knitting ability of bone bracket, induces calcium phosphate active ceramic
The formation of surface bone like apatite layer promotes extracellular response.
(4) macroelement necessary to the human bodies such as sodium ion and potassium ion is provided using sodium carbonate, potassium carbonate.
Specific embodiment
Below with reference to embodiment, further description of the specific embodiments of the present invention, but the content of the present invention not office
It is limited to this.
Embodiment 1:
One, potassium carbonate, sodium carbonate and 3 grams, 2 grams and 1 gram of lithium carbonate powder are weighed respectively, weigh hydroxyapatite powder 94
Gram, totally 100 grams；Then weighed powder is put into be configured in 900 grams of alcohol 10% mixed liquor, by magnetic stirring apparatus with
The rate of 1200r/min stirs 2 hours and is allowed to uniform；
Two, mixed liquor is filtered, is subsequently placed in vacuum oven, it is 8 hours dry under the conditions of 70 DEG C, it is mixed after drying
It closes powder and passes through ball milling again 20 hours, obtain the uniformly mixed composite powder of solid-state；
Three, by obtained composite powder be packed into the auxiliary powder system of selective laser, under nitrogen atmosphere, use diameter for
The laser facula of 0.8mm, the laser power of 7W, the sintering parameters such as scanning speed of 100mm/min are sintered preparation.
Embodiment 2:
One, potassium carbonate, sodium carbonate and 1.5 grams, 1 gram and 0.5 gram of lithium carbonate powder are weighed respectively, weigh tricalcium phosphate powder
97 grams, totally 100 grams；Then weighed powder is put into be configured in 900 grams of alcohol 10% mixed liquor, pass through magnetic stirring apparatus
It is stirred 2 hours with the rate of 1200r/min and is allowed to uniform；
Two, mixed liquor is filtered, is subsequently placed in vacuum oven, it is 8 hours dry under the conditions of 65 DEG C, it is mixed after drying
It closes powder and passes through ball milling again 25 hours, obtain the uniformly mixed composite powder of solid-state；
Three, use diameter for 1mm under nitrogen atmosphere the obtained composite powder loading auxiliary powder system of selective laser
Laser facula, the laser power of 6W, the sintering parameters such as scanning speed of 100mm/min are sintered preparation.
Claims (3)
1. it is a kind of towards calcium phosphate active ceramic bone bracket preparation multiple liquid phase construction method, using potassium carbonate, sodium carbonate and
The formula that three kinds of materials of lithium carbonate are constituted forms multiple liquid phase, solves calcium phosphate active ceramic when selective laser sintering and is sintered
Problem difficult, consistency is low, while decomposing the gas generated using them and forming microcellular structure necessary to bone bracket, preparation
Technique are as follows:
One, potassium carbonate, sodium carbonate and lithium carbonate are mixed to get carbonate powder by certain mass weighing, according still further to certain mass hundred
Divide ratio to weigh calcium phosphate active ceramic powder and carbonate powder respectively, weighed powder in mass ratio 1: 9 is then put into wine
It is configured to 10% mixed liquor in essence, by magnetic stirrer, obtains uniformly mixed mixed liquor；
Two, mixed liquor is filtered, is subsequently placed in vacuum oven, it is 6~8 hours dry under the conditions of 60 DEG C~80 DEG C,
Mixed-powder after drying passes through ball milling 20~30 hours again, obtains the uniformly mixed composite powder of solid-state；
Three, uniformly mixed composite powder is packed into the auxiliary powder system of selective laser uses diameter for 0.8 under nitrogen atmosphere
The scanning speed sintering parameter of the laser facula of~1mm, the laser power of 6~7W, 100~150mm/min is sintered preparation.
2. according to the method described in claim 1, it is characterised in that: potassium carbonate in the carbonate powder, sodium carbonate and
The mass ratio of lithium carbonate is 3: 2: 1.
3. according to the method described in claim 1, it is characterised in that: the magnetic agitation rotating speed is 1500r/min, time
It is 2-3 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510408375.6A CN106334214B (en) | 2015-07-13 | 2015-07-13 | A kind of multiple liquid phase construction method towards the preparation of calcium phosphate active ceramic bone bracket |
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| CN201510408375.6A CN106334214B (en) | 2015-07-13 | 2015-07-13 | A kind of multiple liquid phase construction method towards the preparation of calcium phosphate active ceramic bone bracket |
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| CN106334214B true CN106334214B (en) | 2019-11-12 |
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Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4403268B2 (en) * | 2001-10-21 | 2010-01-27 | 独立行政法人産業技術総合研究所 | Method for producing calcium phosphate porous sintered body and method for producing artificial bone using the same |
| US8147860B2 (en) * | 2005-12-06 | 2012-04-03 | Etex Corporation | Porous calcium phosphate bone material |
| CN103845762B (en) * | 2012-11-29 | 2017-04-12 | 中南大学 | Method for preparing porous bone scaffold by laser and increasing performance by adding zinc oxide |
| CN102989043A (en) * | 2012-12-21 | 2013-03-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of bone cement porous scaffold by taking carbonate or hydrocarbonate as solid foaming agent |
| CN104119072B (en) * | 2013-04-24 | 2016-01-13 | 中南大学 | A kind of method utilizing selective laser sintering synthesis calcium phosphate to prepare bone support |
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