CN109971985A - A kind of preparation method of POROUS TITANIUM - Google Patents

A kind of preparation method of POROUS TITANIUM Download PDF

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CN109971985A
CN109971985A CN201910291568.6A CN201910291568A CN109971985A CN 109971985 A CN109971985 A CN 109971985A CN 201910291568 A CN201910291568 A CN 201910291568A CN 109971985 A CN109971985 A CN 109971985A
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porous titanium
cerium
titanium
preparation
melting
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CN109971985B (en
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唐建成
许苗苗
周松
叶楠
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Nanchang University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/08—Alloys with open or closed pores
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/08—Alloys with open or closed pores
    • C22C1/081—Casting porous metals into porous preform skeleton without foaming
    • C22C1/082—Casting porous metals into porous preform skeleton without foaming with removal of the preform
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/30—Acidic compositions for etching other metallic material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/44—Compositions for etching metallic material from a metallic material substrate of different composition

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a kind of preparation methods of POROUS TITANIUM, its principle is from cerium to mix Titanium according to different mass ratio proportions, after vacuum melting, corrode corrosion and take off cerium for a period of time, with cleaning solution repeated flushing, vacuum drying is prepared into POROUS TITANIUM, compared with prior art, the de- alloyage that the present invention uses prepares POROUS TITANIUM, and simple process is feasible, easy to operate.Titanium alloy containing cerium is prepared using the method for melting, it is dissolved each other completely using titanium and cerium in liquid phase, solid-solution degree minimum feature prepares POROUS TITANIUM, pass through the content for the cerium that control is added, to control the size of porosity, the process of POROUS TITANIUM formation can be effectively controlled in the entrance for avoiding impurity in POROUS TITANIUM forming process.

Description

A kind of preparation method of POROUS TITANIUM
Technical field
The present invention relates to POROUS TITANIUM or titanium alloy field more particularly to a kind of preparation methods of POROUS TITANIUM.
Background technique
As a kind of titanium material with a large amount of holes, POROUS TITANIUM not only has good physical-chemical possessed by fine and close titanium Performance, such as high specific strength, good biocompatibility and excellent corrosion resistance, and the presence of hole is also brought Many special functional characteristics, such as extremely-low density, preferable fluid permeability and bigger specific surface area, these characteristics make Obtaining POROUS TITANIUM has the characteristics that structure and function integration, is widely used in the military projects such as Aeronautics and Astronautics department and chemical industry, smelting The civilian departments such as gold, medicine.In the medical domain being most widely used, due to excellent " one's own object " property, titanium and titanium Alloy in hard tissue repair have be widely applied, compared with fine and close titanium, POROUS TITANIUM in terms of mechanical property with sclerous tissues' phase Match, its perforation pore structure can provide biggish space for growing into for tissue, and flowing for body fluid and nutrition exchange provide it is logical Road, and be conducive to the growth of peripheral cell ingrowing and new bone, reinforce the biological fixation with bone tissue.
The preparation method of POROUS TITANIUM mainly has slurry foaming, powder metallurgic method, casting, SHS process at present Method etc., Y.W.Gu et al. is with TiH2For pore creating material and activator, the method for using powder metallurgy has prepared pore diameter range as 90- 190 μm, the porous titanium alloy of percent opening 43%-59%.Guobo Yang et al. uses calcium steam reduction Ti2O3Hole is prepared Gap rate is the POROUS TITANIUM of 62%-82%, and percent opening is greater than 90%.
How to prepare POROUS TITANIUM using more simple and feasible method is always the target that many scholars explore.
Summary of the invention
The purpose of the present invention is to solve the above-mentioned technical problems in the prior art, provide a kind of system of POROUS TITANIUM Preparation Method, principle are that two kinds of titanium, cerium metals are respectively mutually distributed with independent, uniform after vacuum melting, form pseudo-alloy Phase, makes Ce be separated by acid corrosion, and POROUS TITANIUM is formed by after cleaning-drying without other impurities, and passes through control Ce's The forming process of POROUS TITANIUM can be effectively controlled in additional amount.
In order to achieve the object of the present invention, the technical solution adopted is that, a kind of preparation method of POROUS TITANIUM is designed, includes Following steps:
1) cerium is taken out from kerosene, and is eluted with ethanol solution, by the cerium hair dryer after elution Cold wind drying, it is spare；
2) Titanium is mixed into master alloy according to different mass ratio proportions from the spare cerium of drying in step 1), It is spare；
3) master alloy being equipped in step 2) is subjected to melting under vacuum conditions, titanium cerium two-phase is kept in fusion process It is uniformly mixed；
4) master alloy after melting in step 3) is infiltrated into a period of time until emerging without bubble using corrosive liquid, carried out POROUS TITANIUM stock is formed after corroding de- cerium；
5) the POROUS TITANIUM stock in step 4) is cleaned；
6) the POROUS TITANIUM stock after cleaning in step 5 carries out vacuum drying and is prepared into POROUS TITANIUM.
Preferably, Titanium purity >=99.6%, cerium purity >=99.9%.
Preferably, to prevent cerium rapid oxidation in air, the step 1) is before the step 3) starts It carries out within 10 minutes.
Preferably, in the step 2) Titanium and cerium different quality ratio range be (21: 4)~(10: 15)。
Preferably, the instrument of melting is vacuum arc melting furnace, vacuum degree≤3 × 10 in the step 3)-3Pa。
Preferably, the corrosive liquid in the step 4) is that hydrochloric acid, sulfuric acid or nitric acid that concentration is 5mol/L~10mol/L are molten Liquid.
Preferably, the time corroded in the step 4) is 2-10h.
Preferably, cleaning solution used in the step 5) is deionized water and ethanol solution, the cleaning of the step 5) Step further includes that POROUS TITANIUM stock is put into the beaker equipped with ethanol solution to clean 20min with ultrasonic oscillation instrument.
Preferably, purity >=99.7% of the ethanol solution.
Compared with prior art, the de- alloyage that the present invention uses prepares POROUS TITANIUM, and simple process is feasible, easy to operate. Titanium alloy containing cerium is prepared using the method for melting, is dissolved each other completely using titanium and cerium in liquid phase, the minimum feature of solid-solution degree POROUS TITANIUM is prepared, the content for the cerium being added by control to control the size of porosity avoids POROUS TITANIUM and formed The process of POROUS TITANIUM formation can be effectively controlled in the entrance of impurity in the process.
Detailed description of the invention
The present invention is further described with reference to the accompanying drawing.
Fig. 1 is the scanning electron microscope (SEM) photograph for the POROUS TITANIUM that embodiment 1 is prepared.
Fig. 2 is the XRD diffracting spectrum for the POROUS TITANIUM that embodiment 1 is prepared.
Fig. 3 is the scanning electron microscope (SEM) photograph for the POROUS TITANIUM that embodiment 3 is prepared.
Fig. 4 is the scanning electron microscope (SEM) photograph for the POROUS TITANIUM that embodiment 2 is prepared.
Specific embodiment
Below by specific embodiment combination attached drawing, invention is further described in detail.
Raw material, equipment used in the specific embodiment of the invention are known product, are obtained by purchase commercial product.
The present invention provides one kind mainly using titanium and cerium as primary raw material, and the side of porous titanium material is prepared by taking off alloyage Method.
Embodiment 1
Cerium is taken out from kerosene, is eluted three times using ethanol solution, is dried up with hair dryer cold wind, according to titanium cerium matter Amount is put into vacuum arc melting furnace, vacuum degree≤3 × 10 than carrying out ingredient for 21: 4-3Pa, electric current 250A carry out melting, To keep titanium cerium two-phase mixtures uniform in fusion process, the sample solidified is turned with manipulator and carries out melting again, such as This is reciprocal two to three times.
Master alloy is put into the hydrochloric acid that concentration is 5mol/L after the completion of melting and is corroded, etching time 5h, until not having Bubble is emerged.Corrosion sample is taken out, repeated flushing is distinguished with deionized water and ethanol solution, after flushed, is put into equipped with second 20min is cleaned with ultrasonic oscillation instrument in the beaker of alcoholic solution, cleaning is put into vacuum oven later to be done under the conditions of 120 DEG C Dry 2h.Titanium purity >=99.6% used in above-mentioned steps, cerium purity >=99.9%, ethanol solution purity >= 99.7%.To prevent cerium rapid oxidation in air, takes out and carry out from kerosene within ten minutes before melting experiment starts Cleaning drying.
Referring to Figure 1, Fig. 2, gained POROUS TITANIUM particle diameter distribution are 0.60-2.62 μm, and 1.63 μm of average grain diameter, porosity is 25.40%, hole wall micro-vickers hardness is 250HV.
Embodiment 2
Cerium is taken out from kerosene, is eluted three times using ethanol solution, is dried up with hair dryer cold wind, according to titanium cerium matter Amount is put into vacuum arc melting furnace, vacuum degree≤3 × 10 than carrying out ingredient for 18: 7-3Pa, electric current 250A carry out melting, To keep titanium cerium two-phase mixtures uniform in fusion process, the sample solidified is turned with manipulator and carries out melting again, such as This is reciprocal two to three times.
Master alloy is put into the hydrochloric acid that concentration is 5mol/L after the completion of melting and is corroded, etching time 5h, until not having Bubble is emerged.Corrosion sample is taken out, repeated flushing is distinguished with deionized water and ethanol solution, after flushed, is put into equipped with second 20min is cleaned with ultrasonic oscillation instrument in the beaker of alcoholic solution, cleaning is put into 120 DEG C of dry 2h in vacuum oven later.On State Titanium purity >=99.6% used in step, cerium purity >=99.9%, ethanol solution purity >=99.7%.It is anti- Only cerium rapid oxidation in air takes out from kerosene before melting experiment starts and carries out cleaning drying for ten minutes.
Fig. 3 is referred to, gained POROUS TITANIUM particle diameter distribution is 1.10-4.70 μm, and average grain diameter is 2.16 μm, and porosity is 35.48%, hole wall micro-vickers hardness is 184HV.
Embodiment 3
Cerium is taken out from kerosene, is eluted three times using ethanol solution, is dried up with hair dryer cold wind, according to titanium cerium matter Amount is put into vacuum arc melting furnace, vacuum degree≤3 × 10 than carrying out ingredient for 17: 8-3Pa, electric current 250A carry out melting, To keep titanium cerium two-phase mixtures uniform in fusion process, the sample solidified is turned with manipulator and carries out melting again, such as This is reciprocal two to three times.
Master alloy is put into the hydrochloric acid that concentration is 5mol/L after the completion of melting and is corroded, etching time 5h, until not having Bubble is emerged.Corrosion sample is taken out, repeated flushing is distinguished with deionized water and ethanol solution, after flushed, is put into equipped with second 20min is cleaned with ultrasonic oscillation instrument in the beaker of alcoholic solution, cleaning is put into 120 DEG C of dry 2h in vacuum oven later.On State Titanium purity >=99.6% used in step, cerium purity >=99.9%, ethanol solution purity >=99.7%.It is anti- Only cerium rapid oxidation in air takes out from kerosene before melting experiment starts and carries out cleaning drying for ten minutes.
Fig. 4 is referred to, gained POROUS TITANIUM particle diameter distribution is 0.60-3.67 μm, and average grain diameter is 1.91 μm, and porosity is 57.87%, hole wall micro-vickers hardness is 213HV.
Embodiment 4
Cerium is taken out from kerosene, is eluted three times using ethanol solution, is dried up with hair dryer cold wind, according to titanium cerium matter Amount is put into vacuum arc melting furnace, vacuum degree≤3 × 10 than carrying out ingredient for 10: 15-3Pa, electric current 250A carry out melting, It is uniform for holding titanium cerium two-phase mixtures in fusion process, the sample solidified is turned with manipulator and carries out melting again, And so on two to three times.
Master alloy is put into the hydrochloric acid that concentration is 5mol/L after the completion of melting and is corroded, etching time 5h, until not having Bubble is emerged.Corrosion sample is taken out, repeated flushing is distinguished with deionized water and ethanol solution, after flushed, is put into equipped with second 20min is cleaned with ultrasonic oscillation instrument in the beaker of alcoholic solution, cleaning is put into 120 DEG C of dry 2h in vacuum oven later.On State Titanium purity >=99.6% used in step, cerium purity >=99.9%, ethanol solution purity >=99.7%.It is anti- Only cerium rapid oxidation in air takes out from kerosene before melting experiment starts and carries out cleaning drying for ten minutes.
Gained POROUS TITANIUM particle diameter distribution is 0.26-3.43 μm, and average grain diameter is 1.73 μm, porosity 10.93%, hole wall Micro-vickers hardness is 240HV.
Following table is the obtained POROUS TITANIUM performance evaluation of different titanium cerium quality proportionings:
mTi∶mce Particle diameter distribution/μm Average grain diameter/μm Porosity/% Vickers hardness/HV
21∶4 0.60-2.62 1.63 25.40 250
18∶7 1.10-4.70 2.16 35.48 184
17∶8 0.60-3.67 1.91 57.87 213
15∶10 0.88-3.63 1.72 39.22 219
14∶11 0.36-5.29 1.55 29.57 226
13∶12 1.03-3.63 2.45 17.63 213
10∶15 0.26-3.43 1.73 10.93 240
In the description of this specification, reference term " embodiment ", " some embodiments ", " an implementation The description of example ", " some embodiments ", " example ", " specific example " or " some examples " etc. means to combine the embodiment or example Particular features, structures, materials, or characteristics described are included at least one embodiment or example of the invention.In this explanation In book, schematic expression of the above terms be may not refer to the same embodiment or example.Moreover, the specific spy of description Sign, structure, material or feature can be combined in any suitable manner in any one or more of the embodiments or examples.
The above content is specific embodiment is combined, further detailed description of the invention, and it cannot be said that this hair Bright specific implementation is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, it is not taking off Under the premise of from present inventive concept, a number of simple deductions or replacements can also be made.

Claims (9)

1. a kind of preparation method of POROUS TITANIUM, which is characterized in that comprise the following steps that
1) cerium is taken out from kerosene, and is eluted with ethanol solution, by the hair dryer cold wind of the cerium after elution Drying, it is spare；
2) Titanium is mixed into master alloy according to different mass ratio proportions from the spare cerium of drying in step 1), it is standby With；
3) master alloy being equipped in step 2) is subjected to melting under vacuum conditions, titanium cerium two-phase mixtures are kept in fusion process Uniformly；
4) master alloy after melting in step 3) is infiltrated into a period of time until emerging without bubble using corrosive liquid, is corroded POROUS TITANIUM stock is formed after de- cerium；
5) the POROUS TITANIUM stock in step 4) is cleaned；
6) the POROUS TITANIUM stock after cleaning in step 5 carries out vacuum drying and is prepared into POROUS TITANIUM.
2. a kind of preparation method of POROUS TITANIUM according to claim 1, which is characterized in that the Titanium purity >= 99.6%, cerium purity >=99.9%.
3. a kind of preparation method of POROUS TITANIUM according to claim 1, which is characterized in that prevent the cerium in sky Rapid oxidation in gas, the step 1) start to carry out for first 10 minutes in the step 3).
4. a kind of preparation method of POROUS TITANIUM according to claim 1, which is characterized in that in the step 2) Titanium with Cerium different quality ratio range is (21: 4)~(10: 15).
5. a kind of preparation method of POROUS TITANIUM according to claim 1, which is characterized in that the instrument of melting in the step 3) Device is vacuum arc melting furnace, vacuum degree≤3 × 10-3Pa。
6. a kind of preparation method of POROUS TITANIUM according to claim 1, which is characterized in that the corrosive liquid in the step 4) Hydrochloric acid, sulfuric acid or the nitric acid solution for being 5mol/L~10mol/L for concentration.
7. a kind of preparation method of POROUS TITANIUM according to claim 1, which is characterized in that corrode in the step 4) when Between be 2-10h.
8. a kind of preparation method of POROUS TITANIUM according to claim 1, which is characterized in that clear used in the step 5) Washing lotion is deionized water and ethanol solution, and the cleaning step of the step 5) further includes that POROUS TITANIUM stock is put into equipped with second 20min is cleaned with ultrasonic oscillation instrument in the beaker of alcoholic solution.
9. a kind of preparation method of POROUS TITANIUM according to claim 8, which is characterized in that the purity of the ethanol solution >= 99.7%.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112871125A (en) * 2021-01-05 2021-06-01 南京华东电子真空材料有限公司 Preparation method of high-reliability sheet-shaped getter without risk of particle falling

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07258766A (en) * 1994-03-18 1995-10-09 Mitsubishi Materials Corp Production of molded goods of ti3al intermetallic compound
JP2006083444A (en) * 2004-09-17 2006-03-30 National Institute For Materials Science Porous titanium alloy
KR20150063880A (en) * 2013-12-02 2015-06-10 자동차부품연구원 Hybrid porous body and method of fabricating the same
CN104831104A (en) * 2015-04-03 2015-08-12 东南大学 Preparation method of three dimensional nanometer porous titanium and alloy thereof
CN105149607A (en) * 2015-09-16 2015-12-16 哈尔滨工业大学 Preparation method of nano-porous titanium powder or nano-porous nickel powder
CN105568029A (en) * 2015-11-30 2016-05-11 陕西高新能源发展有限公司 Method for preparing porous titanium

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07258766A (en) * 1994-03-18 1995-10-09 Mitsubishi Materials Corp Production of molded goods of ti3al intermetallic compound
JP2006083444A (en) * 2004-09-17 2006-03-30 National Institute For Materials Science Porous titanium alloy
KR20150063880A (en) * 2013-12-02 2015-06-10 자동차부품연구원 Hybrid porous body and method of fabricating the same
CN104831104A (en) * 2015-04-03 2015-08-12 东南大学 Preparation method of three dimensional nanometer porous titanium and alloy thereof
CN105149607A (en) * 2015-09-16 2015-12-16 哈尔滨工业大学 Preparation method of nano-porous titanium powder or nano-porous nickel powder
CN105568029A (en) * 2015-11-30 2016-05-11 陕西高新能源发展有限公司 Method for preparing porous titanium

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112871125A (en) * 2021-01-05 2021-06-01 南京华东电子真空材料有限公司 Preparation method of high-reliability sheet-shaped getter without risk of particle falling
CN112871125B (en) * 2021-01-05 2023-07-07 南京华东电子真空材料有限公司 Preparation method of flake-shaped getter without particle falling risk

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