CN113416865A - 一种轻质金属发泡材料及其制备方法 - Google Patents
一种轻质金属发泡材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 60
- 239000006262 metallic foam Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 74
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 70
- 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 56
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 39
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000010936 titanium Substances 0.000 claims abstract description 25
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 25
- 239000011261 inert gas Substances 0.000 claims abstract description 22
- 238000001704 evaporation Methods 0.000 claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 16
- 238000005187 foaming Methods 0.000 claims abstract description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 13
- 239000001301 oxygen Substances 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 230000008020 evaporation Effects 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims description 42
- 238000007873 sieving Methods 0.000 claims description 24
- 229910052720 vanadium Inorganic materials 0.000 claims description 22
- 239000000956 alloy Substances 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims 2
- 239000007943 implant Substances 0.000 abstract description 13
- 210000000988 bone and bone Anatomy 0.000 abstract description 11
- 239000011258 core-shell material Substances 0.000 abstract description 4
- 239000000779 smoke Substances 0.000 abstract description 4
- 238000005507 spraying Methods 0.000 abstract description 4
- 230000008021 deposition Effects 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- 238000007740 vapor deposition Methods 0.000 abstract description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 11
- 239000007769 metal material Substances 0.000 description 5
- 208000010392 Bone Fractures Diseases 0.000 description 4
- 241000699670 Mus sp. Species 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002513 implantation Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 208000001132 Osteoporosis Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000011164 ossification Effects 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[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 VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- -1 phosphorus ions Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
- B22F3/1125—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers involving a foaming process
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
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Abstract
本发明公开了一种轻质金属发泡材料及其制备方法,涉及新材料技术领域。本发明先先将钛合金与羟基磷灰石进行蒸发沉积进行初次发泡,再将初次发泡的钛合金‑羟基磷灰石复合物进行热等静压处理;进行蒸汽沉积时先横向喷出惰性气体,使钛合金变为金属烟,再向纵向喷出流速较高的惰性气体,同时向体系中加入羟基磷灰石,再纵向羟基磷灰石烟雾运动下在上方的低温板上,直接形成羟基磷灰石包覆钛合金的球状核壳状钛合金‑羟基磷灰石复合物,热等静压处理时使用惰性气体和氧气作为加压介质,直接制备孔隙率在60~80%的轻质发泡金属。本发明制备的轻质金属发泡材料孔隙率在60~80%,非常适合作为植入体植入骨内。
Description
技术领域
本发明涉及新材料领域,具体为一种轻质金属发泡材料及其制备方法。
背景技术
作为医用植入体植入材料的金属材料,植入后需要具备一定的抗冲击能力才能保证在其植入人体后能承受各种作用力的作用。对于植入物,材料还应具备一定的疲劳强度和高的是耐磨性,以适应长期使用的需要。医用材料的耐磨性是长期植入性材料的一项重要指标。耐磨性差会导致发言、感染、以及植入材料松动等不良后果,最后导致植入物的损坏。
当金属植入人体后,由于人体的运动,必然会与周围的骨组织发生作用,这些作用包括拉压或变弯载荷。这些载荷的作用将会对骨组织造成破坏,如造成组织厚度下降,即骨变薄,以及骨质疏松等,这种现象被成为“应力屏蔽”现象。钛合金一直应用与医用植入领域,且钛合金中的钒能够增强钛合金植入体后的耐磨性,但过量的钒散入体内后会导致钒中毒,钛合金中的钒太少,又会导致植入体力学性能下降。
发明内容
本发明的目的在于提供一种轻质金属发泡材料及其制备方法,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明第一方面提供如下技术方案:一种轻质金属发泡材料的制备方法,其特征在于,制备轻质金属发泡材料的工艺流程为:
钛合金材料制备,羟基磷灰石材料制备,蒸发沉积,热等静压。
优选的,包括以下具体步骤:
(1)将钛合金进行球磨过筛,制得钛合金材料;
(2)将羟基磷灰石进行球磨过筛,制得羟基磷灰石材料;
(3)在真空状态下将钛合金材料与羟基磷灰石材料分别加热至气态,制得蒸发钛合金气与蒸发羟基磷灰石气;向装有真空密封进气系统的钟罩式电阻蒸发镀膜机中进行横向进蒸发钛合金气,3~5min后,进行纵向向上进蒸发羟基磷灰石气,3~5min后降温,在镀膜机上面板收集产物,制得初次发泡的钛合金-羟基磷灰石复合物;
(4)将初次发泡的钛合金-羟基磷灰石复合物转移至热等静压炉中,向热等静压炉中通惰性气体和氧气的混合气进行热等静压处理,制得成品。
优选的,上述步骤(1)中:钛合金成分为5.5~6.5%的铝,4.5~5.5%的钒,其余成分为钛。
优选的,上述步骤(1)中:球磨时间为12~24h;将球磨后的钛合金先过100目筛,再过50目筛,选取50~100目之间的钛合金作为钛合金材料。
优选的,上述步骤(2)中:球磨时间为12~24h;将球磨后的羟基磷灰石先过100目筛,再过50目筛,选取50~100目之间的羟基磷灰石作为羟基磷灰石材料。
优选的,上述步骤(3)中:进蒸发钛合金气速率为2~3L/min;进蒸发羟基磷灰石气速率为4~6L/min;降温至1200~1500℃。
优选的,上述步骤(4)中:在启动热等静压炉进行热等静压处理之前,向炉腔内充入惰性气体,将炉腔内的气压控制在1~2MPa;混合气中通惰性气体和氧气的体积比为10:1~15:1,热等静压时的压力为4~7MPa,保持温度为1200~1500℃,时间为10~20min。
本发明第二方面,一种轻质金属发泡材料的制备方法,其特征在于,所述轻质金属发泡材料的制备方法制得的轻质金属发泡材料,包括以下重量份数的原料:10~20份钛合金、20~40份羟基磷灰石。
优选的,所述钛合金成分为5.5~6.5%的铝,4.5~5.5%的钒,其余成分为钛。
与现有技术相比,本发明所达到的有益效果是:
先将钛合金与羟基磷灰石进行蒸发沉积进行初次发泡,再将初次发泡的钛合金-羟基磷灰石复合物进行热等静压处理;进行蒸汽沉积时先横向喷出惰性气体,钛合金蒸发的同时变成金属烟,再向纵向喷出流速较高的惰性气体,同时向体系中加入羟基磷灰石,再纵向羟基磷灰石烟雾运动下在上方的低温板上,直接形成羟基磷灰石包覆钛合金的球状核壳状钛合金-羟基磷灰石复合物,形成初次发泡且孔隙率90%以上的钛合金-羟基磷灰石复合物;热等静压处理时使用惰性气体和氧气作为加压介质,将球状核壳状钛合金-羟基磷灰石复合物烧结并致密化,核壳状破碎的同时,保证钛合金表面的羟基磷灰石覆盖率适中,减小弹性模量,又使本产品的孔隙率在60~80%,适宜作为植入体植入骨内;且在少量氧气作用下,外侧钛合金生成凝胶状态氧化钛钝化膜,使发泡金属材料外侧组分为凝胶状态氧化钛钝化膜,内部为覆盖羟基磷灰石的发泡钛合金;这种方法可以直接制备孔隙率在60~80%的轻质发泡金属,并且这种结构的轻质发泡金属材料植入人体内进行骨内埋植,外部凝胶状态的氧化膜会先诱导体液中钙、磷离子生成磷灰石,进行损坏部位的骨质生成,破损后内部与钛合金链接羟基磷灰石逐渐分解为骨伤恢复提供材料的同时,会先带动钛合金进行骨伤修复和骨质结合再进行分解,使钛合金与骨伤出连接紧密,加快骨伤恢复的同时,避免了松动和脱落;这种轻质发泡金属非常适宜作为植入体植入骨内。
钛合金的组分为5.5~6.5%的铝,4.5~5.5%的钒,其余成分为钛;传统钛合金中钒的含量仅为3.5~4.5%,这是因为人体中钒的含量较少,外加骨质中钒的含量过多会引起中毒,但较少的钒只是在一定程度上增强钛合金的耐磨性、耐腐蚀和机械性能,经过蒸发沉积和热等静压后的轻质金属发泡材料,更加增强材料的耐磨性、耐腐蚀和机械性能,使轻质金属发泡材料接近人骨的力学性能的同时,钒会优先与材料中羟基磷灰石分解出的无机磷结合,不会扩散到人体中,使制备得到的轻质金属发泡材料接近人骨的力学性能的同时,更加耐磨,更适宜作为植入体植入骨内。
具体实施方式
下面将结合本发明的实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
为了更清楚的说明本发明提供的方法通过以下实施例进行详细说明,在以下实施例中制备的轻质金属发泡材料的各指标测试方法如下:
钒含量:将制备的实施例1、2与对比例1、2植入小鼠体内,三个月后进行体内钒含量测量,小鼠体内钒含量0.25mg/L以上中毒。
实施例1
一种轻质金属发泡材料,按重量份数计,主要包括:
10份的钛合金、20份的羟基磷灰石;
所述钛合金为5.5%的铝,4.5%的钒,其余成分为钛。
一种轻质金属发泡材料的制备,所述轻质金属发泡材料制备方法为:
(1)将钛合金进行球磨过筛,球磨时间为12h,将球磨后的钛合金先过100目筛,再过50目筛,选取50~100目之间的钛合金作为钛合金材料,制得钛合金材料;
(2)将羟基磷灰石进行球磨过筛,球磨时间为12h,将球磨后的羟基磷灰石先过100目筛,再过50目筛,选取50~100目之间的羟基磷灰石作为羟基磷灰石材料,制得羟基磷灰石材料;
(3)在真空状态下将钛合金材料与羟基磷灰石材料分别加热至气态,制得蒸发钛合金气与蒸发羟基磷灰石气;向装有真空密封进气系统的钟罩式电阻蒸发镀膜机中进行横向进蒸发钛合金气,进气速率为2L/min,3min后,进行纵向向上进蒸发羟基磷灰石气,进气速率为4L/min,3min后降温至1200℃,在镀膜机上面板收集产物,制得初次发泡的钛合金-羟基磷灰石复合物;
(4)将初次发泡的钛合金-羟基磷灰石复合物转移至热等静压炉中,向热等静压炉中通惰性气体和氧气的混合气进行热等静压处理,在启动热等静压炉进行热等静压处理之前,向炉腔内充入惰性气体,将炉腔内的气压控制在1MPa,混合气中通惰性气体和氧气的体积比为10:1,热等静压时的压力为4MPa,保持温度为1200℃,时间为10min,冷却至室温,制得成品。
实施例2
一种轻质金属发泡材料,按重量份数计,主要包括:
20份的钛合金、40份的羟基磷灰石;
所述钛合金为6.5%的铝,5.5%的钒,其余成分为钛。
一种轻质金属发泡材料的制备,所述轻质金属发泡材料制备方法为:
(1)将钛合金进行球磨过筛,球磨时间为24h,将球磨后的钛合金先过100目筛,再过50目筛,选取50~100目之间的钛合金作为钛合金材料,制得钛合金材料;
(2)将羟基磷灰石进行球磨过筛,球磨时间为24h,将球磨后的羟基磷灰石先过100目筛,再过50目筛,选取50~100目之间的羟基磷灰石作为羟基磷灰石材料,制得羟基磷灰石材料;
(3)在真空状态下将钛合金材料与羟基磷灰石材料分别加热至气态,制得蒸发钛合金气与蒸发羟基磷灰石气;向装有真空密封进气系统的钟罩式电阻蒸发镀膜机中进行横向进蒸发钛合金气,进气速率为3L/min,4min后,进行纵向向上进蒸发羟基磷灰石气,进气速率为6L/min,4min后降温至1500℃,在镀膜机上面板收集产物,制得初次发泡的钛合金-羟基磷灰石复合物;
(4)将初次发泡的钛合金-羟基磷灰石复合物转移至热等静压炉中,向热等静压炉中通惰性气体和氧气的混合气进行热等静压处理,在启动热等静压炉进行热等静压处理之前,向炉腔内充入惰性气体,将炉腔内的气压控制在2MPa,混合气中通惰性气体和氧气的体积比为15:1,热等静压时的压力为7MPa,保持温度为1500℃,时间为15min,冷却至室温,制得成品。
对比例1
对比例1的处方组成同实施例1。该轻质金属发泡材料的制备方法与实施例1的区别仅在于步骤(3)的不同,将步骤(3)修改为:在真空状态下将钛合金材料与羟基磷灰石材料按质量比1:2混合,并加热至气态,制得蒸发钛合金-羟基磷灰石复合气;向装有真空密封进气系统的钟罩式电阻蒸发镀膜机中进蒸发钛合金-羟基磷灰石复合气,进气速率为2L/min,3min后降温至1200℃,在镀膜机上面板收集产物,制得初次发泡的钛合金-羟基磷灰石复合物。其余制备步骤同实施例1。
对比例2
对比例2的处方组成同实施例1。该轻质金属发泡材料的制备方法与实施例1的区别仅在于步骤(4)的不同,将步骤(4)修改为:(4)将初次发泡的钛合金-羟基磷灰石复合物转移至热等静压炉中,向热等静压炉中通惰性气体进行热等静压处理,在启动热等静压炉进行热等静压处理之前,向炉腔内充入惰性气体,将炉腔内的气压控制在1MPa,热等静压时的压力为4MPa,保持温度为1200℃,时间为10min,冷却至室温,制得成品。其余制备步骤同实施例1。
效果例
下表1给出了采用本发明实施例1、2与对比例1、2、3的轻质金属发泡材料性能分析结果。
表1
孔隙率(%) | 植入后体内钒含量(mg/L) | |
实施例1 | 78.1 | 0.11 |
实施例2 | 75.9 | 0.14 |
对比例1 | 50.1 | 0.55 |
对比例2 | 60.3 | 2.4 |
通过实施例1、2与对比例1、2的孔隙率比较可明显发现,制备的轻质金属发泡材料中分别将钛合金和羟基磷灰石蒸发至蒸气后再混合,与在热等静压时通惰性气体与氧气的混合气都将本产品的孔隙率调节在适合植入人体内的范围内;通过实施例1、2与对比例1、2的孔隙率比较可明显发现制备的轻质金属发泡材料中分别将钛合金和羟基磷灰石蒸发至蒸气后再混合,与在热等静压时通惰性气体与氧气的混合气,都使羟基磷灰石与钒结合,不扩散到体内,使得钒即增强本产品耐磨性的同时,又不会增加人体内钒的含量,使本产品更适合植入人体。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种轻质金属发泡材料的制备方法,其特征在于,制备轻质金属发泡材料的工艺流程为:钛合金材料制备,羟基磷灰石材料制备,蒸发沉积,热等静压。
2.根据权利要求1所述的一种轻质金属发泡材料的制备方法,其特征在于,包括以下具体步骤:
(1)将钛合金进行球磨过筛,制得钛合金材料;
(2)将羟基磷灰石进行球磨过筛,制得羟基磷灰石材料;
(3)在真空状态下将钛合金材料与羟基磷灰石材料分别加热至气态,制得蒸发钛合金气与蒸发羟基磷灰石气;向装有真空密封进气系统的钟罩式电阻蒸发镀膜机中进行横向进蒸发钛合金气,3~5min后,进行纵向向上进蒸发羟基磷灰石气,3~5min后降温,在镀膜机上面板收集产物,制得初次发泡的钛合金-羟基磷灰石复合物;
(4)将初次发泡的钛合金-羟基磷灰石复合物转移至热等静压炉中,向热等静压炉中通惰性气体和氧气的混合气进行热等静压处理,制得成品。
3.根据权利要求2所述的一种轻质金属发泡材料的制备方法,其特征在于,上述步骤(1)中:钛合金成分为5.5~6.5%的铝,4.5~5.5%的钒,其余成分为钛。
4.根据权利要求2所述的一种轻质金属发泡材料的制备方法,其特征在于,上述步骤(1)中:球磨时间为12~24h;将球磨后的钛合金先过100目筛,再过50目筛,选取50~100目之间的钛合金作为钛合金材料。
5.根据权利要求2所述的一种轻质金属发泡材料的制备方法,其特征在于,上述步骤(2)中:球磨时间为12~24h;将球磨后的羟基磷灰石先过100目筛,再过50目筛,选取50~100目之间的羟基磷灰石作为羟基磷灰石材料。
6.根据权利要求2所述的一种轻质金属发泡材料的制备方法,其特征在于,上述步骤(3)中:进蒸发钛合金气速率为2~3L/min;进蒸发羟基磷灰石气速率为4~6L/min;降温至1200~1500℃。
7.根据权利要求2所述的一种轻质金属发泡材料的制备方法,其特征在于,上述步骤(4)中:在启动热等静压炉进行热等静压处理之前,向炉腔内充入惰性气体,将炉腔内的气压控制在1~2MPa;混合气中通惰性气体和氧气的体积比为10:1~15:1,热等静压时的压力为4~7MPa,保持温度为1200~1500℃,时间为10~20min。
8.根据权利要求1所述的一种轻质金属发泡材料的制备方法,其特征在于,所述轻质金属发泡材料的制备方法制得的轻质金属发泡材料,包括以下重量份数的原料:10~20份钛合金、20~40份羟基磷灰石。
9.根据权利要求8所述的一种轻质金属发泡材料的制备方法,其特征在于,所述钛合金成分为5.5~6.5%的铝,4.5~5.5%的钒,其余成分为钛。
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