CN1234602C - Method for in situ synthesis of calcium salt composite powder of bioceramic coating - Google Patents
Method for in situ synthesis of calcium salt composite powder of bioceramic coating Download PDFInfo
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- CN1234602C CN1234602C CN 200310109062 CN200310109062A CN1234602C CN 1234602 C CN1234602 C CN 1234602C CN 200310109062 CN200310109062 CN 200310109062 CN 200310109062 A CN200310109062 A CN 200310109062A CN 1234602 C CN1234602 C CN 1234602C
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Abstract
The present invention a preparation method of calcium salt composite powder of a biological ceramic coating through in-situ synthesis, which belongs to the technical field of material preparation. In the present invention, calcium carbonate CaCO3 and calcium hydrogen phosphate CaHPO4*2H2O2 powder are firstly obtained by weighing and then evenly mixed. After the mixed powder is quietly positioned for more than 24 hours, 50% to 60% of water content in the mixed powder is removed, and then, composite powder is remixed. After the composite powder is quietly positioned for more than 48 hours, the residual water content is removed. Moreover, the prepared powder is put into a mixer and mixed with corundum balls so as to prepare evenly mixed calcium salt composite powder having good fluidity. The calcium salt composite powder prepared by the present invention has the advantages of even mixing, good fluidity and low water content, and can be used in the novel research field of synthesizing bioceramic coatings by a laser pre-coating method, a powder conveying method by laser, a plasma spraying method, etc. The preparation method can be used for raising labor productivity, reducing technological difficulty and optimizing the bioceramic coatings.
Description
Technical field
That the present invention relates to is a kind of preparation method who prepares the calcium salt composite powder, particularly a kind of preparation method of calcium salt composite powder of original position synthesising biological ceramic coating.Belong to field of material preparation.
Background technology
Hydroxyapatite (Ca
10(PO
4)
6(OH)
2, be called for short HAP) and be the important component part of skeleton, be star's product of bioceramic material, its product is mainly used in substituting and repairing of human body bone, tooth.But its intensity is low, the mechanical property of poor toughness has limited its widespread use.Preparation hydroxyl apatite bioceramic coated material has multiple preparation technology on metallic matrix, as plasma spraying, ion sputtering, electrophoretic deposition etc.Plasma spraying is the unique preparation technology who is adopted on the present clinical application goods.But the bio-ceramic coating that above-mentioned technology obtains, the shortcoming of existence mainly is: coating structure pattern and crystalline ununiformity, reduce biocompatibility and stability; The bonding strength of coating and matrix is relatively poor, causes phenomenon such as occur in the clinical application coming off.Find by literature search, open inferior equality people in " Surface and coatings Technology " (surface and coating technology) (1992,58 (2): the article of delivering 123-125) " Laser surface coating of a bioceramic composite layer " (" laser applies and prepares Bioceramic Composite ") this article makes referrals to: the method that adopts manual precoating on the austenite stainless steel substrate, by add binding agent prefabricated the calcium salt composite powder of one deck with certain gradient, behind appropriate technology laser melting coating, obtaining with the calcium phosphate powder is the compound coating of the bioactive ceramics of main component.But the prefabricated employing of this melting and coating process coating is prefabricated cladding process, need to adopt the wet ball grinding method of adding the binding agent polyvinyl alcohol to prepare prefabricated coating paste, the coating of preparation approaches (0.4～0.6mm), prefabricated to metallic matrix the time when coating paste, the flowability of slurry makes the bad control of the homogeneity of coating; Coating must be dried in baking oven, removes moisture; Occur cracking between coating and the matrix easily and form pore; One transition layer is arranged between coating and the matrix, increased operation and the loaded down with trivial details property in the actually operating.
Secondary calcium phosphate causes it mobile poor owing to contain the cause of crystal water (crystal water content is 20.93%) in self molecular structure, and is big with the uniform mixing difficulty of other materials.When at present using the mixed powder of traditional Prepared by Ball Milling secondary calcium phosphate and lime carbonate, raw material powder all bonds on the ball grinder wall, obtain bean dregs shape, mobile extreme difference, fully can not the dispersive mixed powder.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, the preparation method of the calcium salt composite powder of the synthetic preparation of a kind of original position bio-ceramic coating is provided, make that its preparation mixes, good fluidity, water content is low, also be applicable to simultaneously the calcium salt composite powder of automatic powder feeding method laser melting coating and plasma spraying, this preparation method can raise labour productivity, and reduces the loaded down with trivial details and optimization bio-ceramic coating of technology, thereby has solved the above-mentioned deficiency of precoating method technology in the prior art.
The present invention is achieved by the following technical solutions, and the present invention at first takes by weighing lime carbonate CaCO
3With secondary calcium phosphate CaHPO
42H
2The O powder is with lime carbonate CaCO
3With secondary calcium phosphate CaHPO
42H
2The O powder mixes is even, leaves standstill more than 24 hours, makes CaCO
3Can bring into play its dispersion dehydration, remove in the mixed powder 50%～60% moisture, mix composite powder then again, because the mixed powder of this moment has been sloughed most water, stir easily so it mixes to stir than initial mixing, leave standstill more than 48 hours, further strengthen CaCO
3Dehydration, remove remaining moisture, the powder that makes is put into mixer adds the corundum ball and mix, prepare and mix, good fluidity can not absorb the composite powder of moisture in air.Its structure is solid sphere or subsphaeroidal structure, and the powder granule mean diameter is 100 μ m, and size distribution is between 75～125 μ m.
Below the inventive method is further described, its step is as follows:
(1) takes by weighing starting material lime carbonate CaCO
3(200 orders, analytical pure) and secondary calcium phosphate CaHPO
42H
2O (200 orders, analytical pure) powder, wherein, secondary calcium phosphate CaHPO
42H
2The O weight percent is: 70%～80%, and lime carbonate CaCO
3Weight percent is: 30%～20%, and CaHPO
42H
2O puts into container, CaCO
3Then evenly grind CaHPO with hand
42H
2Among the O or with spoon shape thing CaCO
3Stir into CaHPO
42H
2Among the O.
(2) mixed powder that makes in the step (1) is put into worn-out mouthful container, in dry air, place more than 24 hours.The dehydrating amount of mixed powder is 50%～60%.
(3) the prepared composite powder of step (2) contains moisture, and the small portion powder still has slight reunion.Powder under this state is newly mixed with heavy-handed, improve the degree of its dehydration.
(4) powder that step (3) is made places dry air to place more than 48 hours once more, obtains water content and be 7.44% mixed powder.
(5) powder that makes in the step (4) is put into the drum-type mixer and add the corundum ball and mixed 2 hours, prepare and mix, good fluidity, water content is 6.86% calcium salt composite powder.
Preparation method of the present invention has following effect: (1) prepared powder composition range is wide, because laser beam is a high energy beam, to make starting material produce certain ablation in the course of processing, so require starting material on proportioning, very big fluctuation and adjustability will be arranged.(2) prepared powder mixes, good fluidity, and water content is 6.86%, can not absorb moisture in air.(3) structure is solid sphere or subsphaeroidal structure, and the powder granule mean diameter is 100 μ m, and size distribution is between 75～125 μ m, can be as the prefabricated coating of laser, laser automatic powder feeding method, plasma spraying method powder.When (4) not having transition layer between fore-put powder and the matrix, also can generate bio-ceramic coating, combine for chemical metallurgy between coating and the matrix.From the operation of whole technology, operation is few, and technology is simple, is convenient to operation.(5) from being made into originally, cost of material is cheap, and it is convenient to buy.
Embodiment
Content in conjunction with the inventive method provides following examples:
Embodiment 1:
The prepared composition proportioning is 70%CaHPO
42H
2O and 30% CaCO
3The calcium salt mixed powder.Preparation process is as follows:
(1) takes by weighing 70%CaHPO
42H
2O and 30% CaCO
3Powder, the CaHPO 70%
42H
2O puts into container, the CaCO 30%
3Evenly grind CaHPO with hand
42H
2Among the O.
(2) powder that makes in the step (1) is put into the container of opening, be statically placed in and reach 24 hours in the dry air, the dehydrating amount of mixed powder is 50%.
(3) gained mixed powder in the step (2) is stirred again;
(4) powder that step (3) is made is put in the open containers, leaves standstill in dry air 48 hours, and powder moisture is 7.44%.
(5) powder that makes in the step (4) is put into the drum-type mixer and add corundum ball mixing 2 hours.
The gained powder mixes is even, good fluidity, and water content is 6.86%, can not absorb moisture in air.Structure is solid sphere or subsphaeroidal structure, and the powder granule mean diameter is 100 μ m, and size distribution is between 75～125 μ m.The content of HAP phase is about 9.01% in the prepared bio-ceramic coating of laser melting coating, and coating is that chemical metallurgy combines with matrix.
Embodiment 2:
The prepared composition proportioning is 72%CaHPO
42H
2O and 28% CaCO
3The calcium salt mixed powder.Preparation process is as follows:
(1) takes by weighing 72%CaHPO
12H
2O and 28% CaCO
3Powder, the CaHPO 72%
12H
2O puts into container, the CaCO 28%
3Evenly grind CaHPO with hand
12H
2Among the O.
(2) powder that makes in the step (1) is put into the container of opening, be statically placed in and reach 32 hours in the dry air, the dehydrating amount of mixed powder is 60%.
(3) gained mixed powder in the step (2) is stirred again;
(4) powder that step (3) is made is put in the open containers, leaves standstill in dry air 56 hours, and powder moisture is 7.44%.
(5) powder that makes in the step (4) is put into the drum-type mixer and add corundum ball mixing 2 hours.
The gained powder mixes is even, good fluidity, and water content is 6.86%, can not absorb moisture in air.Structure is solid sphere or subsphaeroidal structure, and the powder granule mean diameter is 100 μ m, and size distribution is between 75～125 μ m.The content of HAP phase is about 10.12% in the prepared bio-ceramic coating of laser melting coating, and coating is that chemical metallurgy combines with matrix.
Embodiment 3:
The prepared composition proportioning is 75%CaHPO
42H
2O and 25% CaCO
3The calcium salt mixed powder.Preparation process is as follows:
(1) takes by weighing 75%CaHPO
42H
2O and 25% CaCO
3Powder, the CaHPO 75%
42H
2O puts into container, the CaCO 25%
3With spoon shape thing CaCO
3Stir into CaHPO
42H
2Among the O.
(2) powder that step (1) is made is put into the container of opening, is statically placed in to reach in the dry air more than 26 hours, and the dehydrating amount of mixed powder is 55%.
(3) gained mixed powder in the step (2) is stirred again;
(4) powder that step (3) is made is put in the open containers, leaves standstill in dry air 50 hours, and powder moisture is 7.44%.
(5) powder that makes in the step (4) is put into the drum-type mixer and add corundum ball mixing 2 hours.
The gained powder mixes is even, good fluidity, and water content is 6.86%, can not absorb moisture in air.Structure is solid sphere or subsphaeroidal structure, and the powder granule mean diameter is 100 μ m, and size distribution is between 75～125 μ m.The content of HAP phase is about 10.12% in the prepared bio-ceramic coating of laser melting coating, and coating is that chemical metallurgy combines with matrix.
Embodiment 4:
The prepared composition proportioning is 80%CaHPO
12H
2O and 20% CaCO
3The calcium salt mixed powder.Preparation process is as follows:
(1) takes by weighing 80%CaHPO
42H
2O and 20% CaCO
3Powder, the CaHPO 80%
12H
2Oo puts into container, the CaCO 20%
3Evenly grind CaHPO with hand
42H
2Among the O.
(2) powder that makes in the step (1) is put into the container of opening, be statically placed in and reach 30 hours in the dry air, the dehydrating amount of mixed powder is 58%.
(3) gained mixed powder in the step (2) is stirred again;
(4) powder that step (3) is made is put in the open containers, leaves standstill in dry air 54 hours, and powder moisture is 7.44%.
(5) powder that makes in the step (4) is put into the drum-type mixer and add corundum ball mixing 2 hours.
The gained powder mixes is even, good fluidity, and water content is 6.86%, can not absorb moisture in air.Structure is solid sphere or subsphaeroidal structure, and the powder granule mean diameter is 100 μ m, and size distribution is between 75～125 μ m.The content of HAP phase is about 50.23% in the prepared bio-ceramic coating of laser melting coating, and coating is that chemical metallurgy combines with matrix.
Claims (2)
1, a kind of preparation method of calcium salt composite powder of original position synthesising biological ceramic coating is characterized in that, its step is as follows:
(1) takes by weighing starting material CaHPO
42H
2O and CaCO
3, wherein, secondary calcium phosphate CaHPO
42H
2The O weight percent is: 70%～80%, and lime carbonate CaCO
3Weight percent is: 30%～20%, and the both is 200 orders, analytical pure, CaHPO
42H
2O puts into container, CaCO
3Then evenly grind CaHPO with hand
42H
2Among the O or with spoon shape thing CaCO
3Stir into CaHPO
42H
2Among the O;
(2) mixed powder that makes in the step (1) is put into open container, place more than 24 hours in dry air, the dehydrating amount of mixed powder is 50%～60%;
(3) the prepared composite powder of step (2) contains moisture, and the small portion powder still has slight reunion, and the powder under this state is newly mixed with heavy-handed;
(4) powder that step (3) is made places dry air to place more than 48 hours once more, obtains water content and be 7.44% mixed powder;
(5) powder that makes in the step (4) is put into the drum-type mixer and add the corundum ball and mixed 2 hours, prepare and mix, good fluidity, water content is 6.86% calcium salt composite powder.
2, the preparation method of the calcium salt composite powder of original position synthesising biological ceramic coating according to claim 1, it is characterized in that, prepared calcium salt composite powder, structure is solid sphere or subsphaeroidal structure, the powder granule mean diameter is 100 μ m, and size distribution is between 75～125 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310109062 CN1234602C (en) | 2003-12-04 | 2003-12-04 | Method for in situ synthesis of calcium salt composite powder of bioceramic coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310109062 CN1234602C (en) | 2003-12-04 | 2003-12-04 | Method for in situ synthesis of calcium salt composite powder of bioceramic coating |
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| Publication Number | Publication Date |
|---|---|
| CN1546372A CN1546372A (en) | 2004-11-17 |
| CN1234602C true CN1234602C (en) | 2006-01-04 |
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|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100457972C (en) * | 2005-09-29 | 2009-02-04 | 上海交通大学 | Production of composite biological ceramic coating by laser coating home position |
| CN100358832C (en) * | 2005-11-22 | 2008-01-02 | 武汉理工大学 | Mullite whisker-mullite composite coating and preparation process thereof |
| CN102031518A (en) * | 2010-12-30 | 2011-04-27 | 同济大学 | method for preparing material with biological ceramic composite coating laser-clad on surface of titanium alloy |
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