CN102031518A - method for preparing material with biological ceramic composite coating laser-clad on surface of titanium alloy - Google Patents

method for preparing material with biological ceramic composite coating laser-clad on surface of titanium alloy Download PDF

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CN102031518A
CN102031518A CN 201010618073 CN201010618073A CN102031518A CN 102031518 A CN102031518 A CN 102031518A CN 201010618073 CN201010618073 CN 201010618073 CN 201010618073 A CN201010618073 A CN 201010618073A CN 102031518 A CN102031518 A CN 102031518A
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titanium alloy
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powder
calcium salt
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王迎春
黄文旵
姚爱华
肖伟
王德平
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Tongji University
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Abstract

The invention relates to a method for preparing biological ceramic composite coating laser-clad on the surface of a titanium alloy, comprising the following steps of: firstly preparing calcium salt composite powder which is mixed uniformly and has good flowability and low water content; then directly stacking the calcium salt composite powder on the surface of a titanium alloy substrate to form a preset coating under the condition of not adding cementing agents; and finally cladding the mixed powder by using laser so as to obtain the material with biological ceramic composite coating on the surface of a titanium alloy. In the invention, a composite biological ceramic coating with uniform texture and good crystallization property can be prepared on the surface of the titanium alloy and, the bond between the coating and the substrate has high strength and belongs to chemical metallurgical bond, thereby solving the problem that the biological ceramic coating is easy to desquamate in a human body; in the invention, used raw materials have low price, are convenient to purchase and easy to store, and are not doped with rare earth components; in addition, the method disclosed in the invention has simple and convenient process, is easy to implement and has good market application prospect and commercial value.

Description

Titanium alloy surface laser melting coating Bioceramic Composite preparation methods
Technical field
The invention belongs to the bioceramic material field, relate to a kind of Bioceramic Composite preparation methods.
Background technology
The bioceramic material that human body hard tissue often uses has zirconium white, aluminum oxide, carbon, bioactivity glass, hydroxyapatite, calcium phosphate etc.In these materials, the sintering bioceramic material has unreactiveness, and is corrosion-resistant, biocompatibility and the stability in Physiological Medium.Hydroxyapatite (the Ca that has particularly come out since the seventies 10(PO 4) 6(OH) 2, HAP) the medical bio pottery is at present both at home and abroad just at flourish biomaterial.Embedded material by the preparation of HAP micro-crystalline ceramic can combine with human body natural's bone is good, is the best bioceramic material of having found of biocompatibility.The biological ceramics of calcium orthophosphate base is the most extensive in clinical application at present, and its main products is HAP, tricalcium phosphate (Ca 3(PO 4) 2, TCP), Calcium Pyrophosphate (β-Ca 2P 2O 7, β-TTCP) etc.Tricalcium phosphate, Calcium Pyrophosphate have good bone inducibility, are a kind of ideal degradable biological stupaliths, and physiological functions such as its bone formation performance are very near HAP.The comprehensive physiological property of the matrix material of HAP and degradable biological pottery will be better than single HAP biological ceramics.The intensity of calcium phosphate ceramic is low, the mechanical property of poor toughness has limited its widespread use.Preparation hydroxyl apatite bioceramic coated material is present domestic and international ongoing research focus on metallic matrix, and plasma spraying is the unique preparation technology who is adopted on the present clinical application goods.The main drawback of the bio-ceramic coating of plasma spraying method preparation can be summarized as:
1. the tissue of coating and degree of crystallinity are inhomogeneous, will reduce biological compatibility of coating and stability;
2. the cohesive strength of coating and matrix is relatively poor, will make coating peel off in clinical application.
At the problems referred to above that hydroxyl apatite bioceramic coating and plasma spray coating process still exist, the calcium phosphorus based biologic active ceramic coating that contains HAP with the laser melting and coating process preparation is developed in recent years.According to the difference of starting material, preparation laser apparatus, the research that at present domestic and international laser melting coating prepares Bioceramic Composite is divided into two main research directions:
1. using the Nd-YAG laser apparatus, is the raw material preparing bio-ceramic coating with HAP.Mainly be the research that the foreign scholar is engaged in this direction at present.Find F. by literature search
Figure BDA0000041984360000011
The article of on " Journal of Materials Science:Materialsin Medicine " magazine 2006 the 17th volume, delivering Deng the people " In vitro testing of Nd:YAG laser processedcalcium phosphate coatings " (the external biological Study on Compatibility of Nd:YAG Laser Clad Bioceramic Coating), this article is introduced: what Nd:YAG laser melting coating starting material adopted is the HAP powder, the bio-ceramic coating of preparation is HAP and TCP composite boilogical ceramic coating, has good biocompatibility.But what these technology starting material adopted is the HAP powder, so cost is higher; In the laser cladding process, the easy decomposes of HAP powder, the content of HAP is restricted in the gained coating.
2. use CO 2Laser apparatus is with CaHPO 42H 2O, CaCO 3And a spot of rare earth composition mixed powder is starting material, and laser melting coating prepares Bioceramic Composite.
Use CO 2Laser apparatus is with CaHPO 42H 2O and CaCO 3Mixed powder when being starting material, must in mixed powder, add rare earth composition (Y 2O 3Or CeO 2), could in cladding layer, obtain comprising the Bioceramic Composite of HAP composition.Find by literature search, the article " Microstructure and osteoblast response of gradient bioceramic coating on titanium alloyfabricated by laser cladding " that people such as Fan Ding delivered on the volume at Applied Surface Science magazine in 2008 the 255th (tissue of titanium alloy surface laser melting coating gradient bio-ceramic coating and sclerocyte reaction "), CO is used in this article introduction 2Laser apparatus is with CaHPO 42H 2O and CaCO 3Mixed powder be starting material, in mixed powder, add rare earth composition CeO 2, could in cladding layer, obtain the Bioceramic Composite that comprises HAP of suitable component.But because this mixed powder is to CO 2The specific absorption of laser is very high, not only makes CaHPO 42H 2O take place to decompose and scaling loss, makes CaHPO in the conventional chemical reaction process 42H 2O and CaCO 3Reaction ratio changes 80% and 20% (wt%) into by 72% and 28% (wt%, weight percent); The laser cladding process temperature is too high simultaneously, and thermodynamics of reactions and reaction kinetics are unfavorable for the generation of HAP, so the content of HAP is restricted in the coating.
The wavelength of Nd:YAG solid statelaser is 1.064 μ m, with CO 2Gas laser (wavelength is 10.64 μ m) is compared, and the wavelength of its output is shorter.But for metallic substance, optical maser wavelength is short more, uptake factor big more (a and b place among the figure), but for pottery and glass material (A and B place among the figure), situation is just in time opposite, as shown in Figure 1, so (1) works as CO 2Laser melting coating CaHPO 42H 2O and CaCO 3When mixed powder prepared bio-ceramic coating, mixed powder was to CO 2The specific absorption of laser will be higher than metallic matrix, CaHPO far away 42H 2O takes place to ablate or decompose; Only in mixed powder, add rare earth composition simultaneously, just can prepare the bio-ceramic coating that main component is HAP; In contrast, during Nd-YAG laser melting coating mixed powder, metallic matrix will be higher than mixed powder far away to the specific absorption of Nd-YAG laser.The contriver has observed Nd-YAG laser for CaHPO in the laser melting coating experiment in early stage 42H 2O and CaCO 3Characteristics with perviousness.(2) transmission ofenergy mode: in the Nd-YAG laser cladding process, the energy of mixed powder synthesising biological pottery is from absorption of N d-YAG laser beam energy and the molten metal matrix, and this existence for HAP in the laser cladding process provides processing and thermodynamic condition.
Summary of the invention
The objective of the invention is to prepare the deficiency of HAP coating, CO at existing plasma spray coating process 2Laser melting coating prepares the deficiency of bio-ceramic coating, is the deficiency that raw-material Nd:YAG laser melting and coating process prepares bio-ceramic coating with HAP, provides a kind of directly with CaHPO 42H 2O and CaCO 3Mixed powder be the laser melting coating preparation method of the simple composite boilogical ceramic coated material of starting material manufacture craft.
Method among the present invention is with low cost; Do not add rare earth composition, and the bio-ceramic coating tissue topography of preparation is even, crystal property is good; The thing phase composite of coating is reasonable, and the composite boilogical ceramic coating for the HAP of stable in properties and degradable tricalcium phosphate, Calcium Pyrophosphate has excellent biological compatibility; The preparation coating is that the high chemical metallurgy of bonding strength combines with matrix, is 25～38Mpa, can solve the problem that bio-ceramic coating peels off in clinical application, and the thickness that this method prepares coating can obtain bigger scope 0～2mm.
For achieving the above object, the present invention is achieved by the following technical solutions:
The calcium salt composite powder is to unique absorption characteristics of Nd-YAG laser, and the water content of powder is qualified simultaneously, and during the laser melting coating mixed powder, metallic matrix will be higher than mixed powder far away to the specific absorption of Nd-YAG laser.The most energy of laser will be absorbed by the metallic surface thin layer in the laser processing procedure, the preset coating energy will be from the metallic surface thin layer of melted state, under suitable photothermal laser mechanics and photochemical effect, calcium salt composite powder and metal base surface thin layer are 10 -6～10 -9, fusing in second.Under suitable laser technical parameters, because high energy laser beam YAG laser apparatus (its wavelength is 1.06 μ m) has unique thermodynamics of reactions and reacting dynamics condition in laser processing procedure, the calcium salt composite powder obtains suitable thermodynamics of reactions and reacting dynamics condition, and the original position synthetic ingredient is HAP/ tricalcium phosphate/β-Ca 2P 2O 7The composite boilogical ceramic coating, coating is that chemical metallurgy combines with matrix, the bonding strength height is 25～38Mpa.Thereby make calcium salt composite powder reaction in generate HAP/ tricalcium phosphate/β-Ca 2P 2O 7Be the composite boilogical ceramic coating of main component, coating presents fibre-reinforced microstructure, and biocompatibility is good.
A kind of titanium alloy surface laser melting coating Bioceramic Composite preparation methods comprises step:
(1) at first preparation mix, good fluidity, calcium salt composite powder that water content is low;
(2) the calcium salt composite powder in the step (1) under the situation of adding additives not directly heap be overlying on titanium alloy-based surface and form preset coating;
(3) laser melting coating mixed powder obtains titanium alloy surface Bioceramic Composite material.
Described titanium alloy substrate is biological medical titanium alloys such as Ti6Al4V, Ti-5Al-2.5Fe, Ti-6Al-7Nb, Ti-13Nb-13Zr, Ti-12Nb-6Zr-2Fe.
The thickness of described preset coating is 0～2mm.
The preparation method of described calcium salt composite powder is: with CaHPO 42H 2O and CaCO 3Mix put into according to a certain percentage open containers mix, leave standstill dehydration, mix again, leave standstill strengthen dewater, mixer mixes, and makes the calcium salt composite powder.
Described CaHPO 42H 2O and CaCO 3Weight percent be: 70%: 30%～75%: 25%.
The average particle diameter of described calcium salt composite powder is 50～100 μ m, and the water content of this powder is 5.8～6.8%.
The processing parameter condition of described laser melting coating is: shielding gas is an argon gas, spot diameter 3mm, output rating 900～1200W, scanning speed 1～3mm/s.
Described laser technical parameters is preferably: fixed light spot size 3mm, scanning speed 1mm/s, laser output power 1200W.
Described laser is the Nd-YAG laser that high energy laser beam iLS-YC-30A YAG type laser apparatus sends, and its wavelength is 1.06 μ m.
The thing phase composite of described coating is: the volume fraction of HAP is 20～61%, and all the other are TCP and β-Ca 2P 2O 7Mixture.
At fixed light spot size 3mm, scanning speed is fixed one of (can among 1～3mm/s), and along with the increase of output rating, the content of HAP increases in the cladding layer, and the microhardness of bio-ceramic coating increases.At fixed light spot size 3mm, output rating is fixed one of (can among 800～1200W), and along with the increase of scanning speed, the content of HAP reduces in the cladding layer, and the microhardness of bio-ceramic coating reduces.Strict gated sweep speed, laser output power, spot size is that the phase composite of acquisition thing is reasonable, dense structure is tiny, microhardness height, the key of the titanium alloy surface Nd-YAG laser melting coating Bioceramic Composite of biocompatibility excellence.Laser cladding process floating coat thickness can be regulated in 0～2mm according to product requirement, is not subjected to the influence of processing parameter.
Preparation method of the present invention has following beneficial effect:
(1) since Nd-YAG laser to CaHPO 42H 2O and CaCO 3Mixed powder has the characteristics of perviousness, so in the Ti6Al4V titanium alloy surface Nd-YAG laser cladding process, the calcium salt mixed powder can obtain to prepare the thermodynamics of reactions and the reaction kinetics of the uniqueness of HAP biological ceramics, so can prepare homogeneous microstructure, composite boilogical ceramic coating that crystal property is good at titanium alloy surface; (2) main component of coating is the composite boilogical ceramic of hydroxyapatite, tricalcium phosphate and the degradable Calcium Pyrophosphate of stable in properties, the biocompatibility excellence; (3) coating and substrate combinating strength height are the chemical metallurgy combination, can solve the problem that bio-ceramic coating comes off in human body easily; (4) from making, cost of material is cheap, and it is convenient to buy, and is easy to store; Need not add rare earth composition in the starting material; Technology is simple and convenient, and is easy to implement, has better market prospect and commercial value.
Description of drawings
Fig. 1 is the specific absorption synoptic diagram of material to different wavelength of laser.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
The thing phase composite of coating is 31%HAP (volume percent), and its excess is TCP and β-Ca mutually 2P 2O 7Mixture, thickness 0.5mm is that chemical metallurgy combines with matrix, bonding strength is the preparation of the Bioceramic Composite of 25～38Mpa.
(1) weighing composition proportion is 72%CaHPO 42H 2O and 28%CaCO 3Above-mentioned powder put into open containers through mix, leave standstill dehydration, mix again, leave standstill strengthen dehydration, mixer mixes, preparing average particle diameter is 50～100 μ m, water content is 6.2% calcium salt composite powder.
(2) calcium salt composite powder heap is overlying on the Ti6Al4V alloy substrate thickness 0.5mm.
(3) be argon gas at shielding gas; spot diameter 3mm, output rating 900W is under the processing parameter of scanning speed 2mm/s; with the Nd-YAG high energy laser beam cladding powder and metallic matrix are carried out the laser melting and coating process processing, form titanium alloy surface Nd-YAG laser melting coating Bioceramic Composite.The coating structure that obtains is even, and crystal property is good, and coat-thickness 0.5mm is that chemical metallurgy combines with matrix, and bonding strength is 25～38Mpa, and the thing phase composite of coating is 31%HAP (volume percent), and its excess is TCP and β-Ca mutually 2P 2O 7Mixture.
Embodiment 2
The thing phase composite of coating is 38%HAP (volume percent), and its excess is TCP and β-Ca mutually 2P 2O 7Mixture, thickness 1mm is that chemical metallurgy combines with matrix, bonding strength is the preparation of the Bioceramic Composite of 25～38Mpa.
(1) weighing composition proportion is 72%CaHPO 42H 2O and 28%CaCO 3Above-mentioned powder put into open containers through mix, leave standstill dehydration, mix again, leave standstill strengthen dehydration, mixer mixes, preparing average particle diameter is that 50～100 μ m water content are 6.2% calcium salt composite powder.
(2) calcium salt composite powder heap is overlying on the Ti6Al4V alloy substrate thickness 1mm.
(3) at spot diameter 3mm, output rating 1000W, under the processing parameter of scanning speed 2mm/s, utilize the Nd-YAG high energy laser beam that cladding powder and metallic matrix are carried out the laser melting and coating process processing, form titanium alloy surface Nd-YAG laser melting coating Bioceramic Composite.The coating structure that obtains is even, and crystal property is good, is that chemical metallurgy combines with matrix, and bonding strength is 25～38Mpa, and the thing phase composite of coating floating coat is 38%HAP (volume percent), and its excess is TCP and β-Ca mutually 2P 2O 7Mixture.
Embodiment 3
The thing phase composite of coating is 47%HAP (volume percent), and its excess is TCP and β-Ca mutually 2P 2O 7Mixture, thickness 1.5mm is that chemical metallurgy combines with matrix, bonding strength is the preparation of the Bioceramic Composite of 25～38Mpa.
(1) weighing composition proportion is 72%CaHPO 42H 2O and 28%CaCO 3Above-mentioned powder put into open containers through mix, leave standstill dehydration, mix again, leave standstill strengthen dehydration, mixer mixes, preparing average particle diameter is that 50～100 μ m water content are 6.2% calcium salt composite powder.
(2) calcium salt composite powder heap is overlying on the Ti6Al4V alloy substrate thickness 1.5mm.
(3) at spot diameter 3mm, output rating 1200W under the processing parameter of scanning speed 2mm/s, can obtain suitable reaction kinetics and thermodynamics of reactions.Utilize the Nd-YAG high energy laser beam that cladding powder and metallic matrix are carried out Laser Cladding Treatment, form titanium alloy surface Nd-YAG laser melting coating Bioceramic Composite.The coating structure that obtains is even, and crystal property is good, is that chemical metallurgy combines with matrix, and bonding strength is 25～38Mpa, and the thing phase composite of coating floating coat is 47%HAP (volume percent), and its excess is TCP and β-Ca mutually 2P 2O 7Mixture.
Embodiment 4
The thing phase composite of coating is 53%HAP (volume percent), and its excess is TCP and β-Ca mutually 2P 2O 7Mixture, thickness 2mm is that chemical metallurgy combines with matrix, bonding strength is the preparation of the Bioceramic Composite of 25～38Mpa.
(1) weighing composition proportion is 72%CaHPO 42H 2O and 28%CaCO 3Above-mentioned powder is put into open containers through mixing, leave standstill dehydration, mixing again, leave standstill and strengthen dehydration, and mixer mixes, and preparing average particle diameter is 50～100 μ m, and water content is 6.2% calcium salt composite powder.
(2) calcium salt composite powder heap is overlying on the Ti6Al4V alloy substrate thickness 2mm.
(3) at spot diameter 3mm, output rating 1000W under the processing parameter of scanning speed 1mm/s, can obtain suitable reaction kinetics and thermodynamics of reactions.Utilize the Nd-YAG high energy laser beam that cladding powder and metallic matrix are carried out the laser melting and coating process processing, form titanium alloy surface Nd-YAG laser melting coating Bioceramic Composite cladding coating.The coating structure that obtains is even, and crystal property is good, and thickness 2mm is that chemical metallurgy combines with matrix, and bonding strength is 25～38Mpa, and the thing phase composite of coating is 53%HAP (volume percent), and its excess is TCP and β-Ca mutually 2P 2O 7Mixture.
Embodiment 5
The thing phase composite of coating is 61%HAP (volume percent), and its excess is TCP and β-Ca mutually 2P 2O 7Mixture, thickness 2mm is that chemical metallurgy combines with matrix, bonding strength is the preparation of the Bioceramic Composite of 25-38Mpa.
(1) weighing composition proportion is 72%CaHPO 42H 2O and 28%CaCO 3Above-mentioned powder is put into open containers through mixing, leave standstill dehydration, mixing again, leave standstill and strengthen dehydration, and mixer mixes, and preparing average particle diameter is 50～100 μ m, and water content is 6.2% calcium salt composite powder.
(2) calcium salt composite powder heap is overlying on the Ti6Al4V alloy substrate thickness 2mm.
(3) at spot diameter 3mm, output rating 1200W under the processing parameter of scanning speed 1mm/s, can obtain suitable reaction kinetics and thermodynamics of reactions.Utilize the Nd-YAG high energy laser beam that cladding powder and metallic matrix are carried out the laser melting and coating process processing, form titanium alloy surface Nd-YAG laser melting coating Bioceramic Composite.The Bioceramic Composite homogeneous microstructure that obtains, crystal property is good, and thickness 2mm is that chemical metallurgy combines with matrix, and bonding strength is 25～38Mpa, and the thing phase composite of coating is 61%HAP (volume percent), its excess is TCP and β-Ca mutually 2P 2O 7Mixture.
At fixed light spot size 3mm, scanning speed is fixed one of (can among 1～3mm/s), and along with the increase of output rating, the content of HAP increases in the cladding layer, and the microhardness of bio-ceramic coating increases.At fixed light spot size 3mm, output rating is fixed one of (can among 800～1200W), and along with the increase of scanning speed, the content of HAP reduces in the cladding layer, and the microhardness of bio-ceramic coating reduces.Strict gated sweep speed, laser output power, spot size is that the phase composite of acquisition thing is reasonable, dense structure is tiny, microhardness height, the key of the titanium alloy surface Nd-YAG laser melting coating Bioceramic Composite of biocompatibility excellence.Laser cladding process floating coat thickness can be regulated in 0～2mm according to product requirement, is not subjected to the influence of processing parameter.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not breaking away from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.

Claims (10)

1. titanium alloy surface laser melting coating Bioceramic Composite preparation methods is characterized in that: comprise step:
(1) at first preparation mix, good fluidity, calcium salt composite powder that water content is low;
(2) the calcium salt composite powder in the step (1) under the situation of adding additives not directly heap be overlying on titanium alloy-based surface and form preset coating;
(3) laser melting coating mixed powder obtains titanium alloy surface Bioceramic Composite material.
2. method according to claim 1 is characterized in that: described titanium alloy substrate is Ti6Al4V, Ti-5Al-2.5Fe, Ti-6Al-7Nb, Ti-13Nb-13Zr or Ti-12Nb-6Zr-2Fe.
3. method according to claim 1 is characterized in that: the thickness of described preset coating is 0-2mm.
4. method according to claim 1 is characterized in that: the preparation method of described calcium salt composite powder is: with CaHPO 42H 2O and CaCO 3Mix put into according to a certain percentage open containers mix, leave standstill dehydration, mix again, leave standstill strengthen dewater, mixer mixes, and makes the calcium salt composite powder.
5. method according to claim 4 is characterized in that: described CaHPO 42H 2O and CaCO 3Weight percent be: 70%: 30%～75%: 25%.
6. method according to claim 1 is characterized in that: the average particle diameter of described calcium salt composite powder is 50-100 μ m, and the water content of this powder is 5.8～6.8%.
7. method according to claim 1 is characterized in that: the processing parameter condition of described laser melting coating is: shielding gas is an argon gas, spot diameter 3mm, output rating 900～1200W, scanning speed 1～3mm/s.
8. method according to claim 1 is characterized in that: described laser is the Nd-YAG laser that high energy laser beam iLS-YC-30A YAG type laser apparatus sends, and its wavelength is 1.06 μ m.
9. method according to claim 1 is characterized in that: the thing phase composite of described coating is: hydroxyapatite, tricalcium phosphate and Calcium Pyrophosphate.
10. method according to claim 9 is characterized in that: the volume fraction of described hydroxyapatite is 20～61%, and all the other are the mixture of tricalcium phosphate and Calcium Pyrophosphate.
CN 201010618073 2010-12-30 2010-12-30 method for preparing material with biological ceramic composite coating laser-clad on surface of titanium alloy Pending CN102031518A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN103422089A (en) * 2013-07-23 2013-12-04 河南工业大学 Nd-YAG laser cladding method for preparing thickness adjustable biological ceramic composite coating adopting bone-like structure
CN104857562A (en) * 2015-04-21 2015-08-26 昆明理工大学 Titanium alloy / calcium pyrophosphate surface bio-composite material and preparation method thereof
CN107233618A (en) * 2017-06-30 2017-10-10 湖北大学 A kind of method that Ag/ZnO/HA nano-composite coatings are prepared on titanium alloy
CN107349472A (en) * 2017-06-30 2017-11-17 浙江德康医疗器械有限公司 A kind of preparation method of the gradient porous titanium alloy of repetition of promotion bone fusion
CN107570876A (en) * 2017-10-16 2018-01-12 江南大学 A kind of processing method of induced with laser KOH chemical reactions etching and cutting sapphire
CN113816770A (en) * 2021-06-25 2021-12-21 西北工业大学 Preparation method for improving surface activity of aluminum oxide-zirconium oxide composite ceramic

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103422089A (en) * 2013-07-23 2013-12-04 河南工业大学 Nd-YAG laser cladding method for preparing thickness adjustable biological ceramic composite coating adopting bone-like structure
CN104857562A (en) * 2015-04-21 2015-08-26 昆明理工大学 Titanium alloy / calcium pyrophosphate surface bio-composite material and preparation method thereof
CN107233618A (en) * 2017-06-30 2017-10-10 湖北大学 A kind of method that Ag/ZnO/HA nano-composite coatings are prepared on titanium alloy
CN107349472A (en) * 2017-06-30 2017-11-17 浙江德康医疗器械有限公司 A kind of preparation method of the gradient porous titanium alloy of repetition of promotion bone fusion
CN107349472B (en) * 2017-06-30 2020-06-30 浙江德康医疗器械有限公司 Preparation method of repeated gradient porous titanium alloy for promoting bone fusion
CN107570876A (en) * 2017-10-16 2018-01-12 江南大学 A kind of processing method of induced with laser KOH chemical reactions etching and cutting sapphire
CN113816770A (en) * 2021-06-25 2021-12-21 西北工业大学 Preparation method for improving surface activity of aluminum oxide-zirconium oxide composite ceramic

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