CN106938336B - A kind of preparation method of magnesium-base porous compound material - Google Patents
A kind of preparation method of magnesium-base porous compound material Download PDFInfo
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- CN106938336B CN106938336B CN201710194891.2A CN201710194891A CN106938336B CN 106938336 B CN106938336 B CN 106938336B CN 201710194891 A CN201710194891 A CN 201710194891A CN 106938336 B CN106938336 B CN 106938336B
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- calcium phosphate
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- 239000000463 material Substances 0.000 title claims abstract description 46
- 150000001875 compounds Chemical class 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000001506 calcium phosphate Substances 0.000 claims abstract description 42
- 229910000389 calcium phosphate Inorganic materials 0.000 claims abstract description 42
- 235000011010 calcium phosphates Nutrition 0.000 claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 42
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims abstract description 42
- 238000005245 sintering Methods 0.000 claims abstract description 34
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000011780 sodium chloride Substances 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 239000011148 porous material Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- UQCVYEFSQYEJOJ-UHFFFAOYSA-N [Mg].[Zn].[Zr] Chemical compound [Mg].[Zn].[Zr] UQCVYEFSQYEJOJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 45
- 239000010439 graphite Substances 0.000 claims description 45
- 229910002804 graphite Inorganic materials 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 45
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 229910001868 water Inorganic materials 0.000 claims description 33
- 239000002585 base Substances 0.000 claims description 29
- PGTXKIZLOWULDJ-UHFFFAOYSA-N [Mg].[Zn] Chemical compound [Mg].[Zn] PGTXKIZLOWULDJ-UHFFFAOYSA-N 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 23
- 239000011812 mixed powder Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 229910052726 zirconium Inorganic materials 0.000 claims description 14
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000012065 filter cake Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 12
- 229910001093 Zr alloy Inorganic materials 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 11
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 10
- 239000001632 sodium acetate Substances 0.000 claims description 10
- 235000017281 sodium acetate Nutrition 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 10
- 229960001763 zinc sulfate Drugs 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 8
- 239000008187 granular material Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 6
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 6
- 229960001484 edetic acid Drugs 0.000 claims description 6
- 235000002906 tartaric acid Nutrition 0.000 claims description 6
- 239000011975 tartaric acid Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical group C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 5
- 238000004826 seaming Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000012512 characterization method Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000007088 Archimedes method Methods 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- 230000003001 depressive effect Effects 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- 239000011888 foil Substances 0.000 claims description 2
- 238000005246 galvanizing Methods 0.000 claims description 2
- 239000007770 graphite material Substances 0.000 claims description 2
- 238000000265 homogenisation Methods 0.000 claims description 2
- 239000002932 luster Substances 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 230000000717 retained effect Effects 0.000 claims description 2
- 229910000144 sodium(I) superoxide Inorganic materials 0.000 claims description 2
- 239000007779 soft material Substances 0.000 claims description 2
- 238000004611 spectroscopical analysis Methods 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000003860 storage Methods 0.000 claims description 2
- 230000003746 surface roughness Effects 0.000 claims description 2
- 229960001367 tartaric acid Drugs 0.000 claims description 2
- 238000012360 testing method Methods 0.000 claims description 2
- 229910000391 tricalcium phosphate Inorganic materials 0.000 claims description 2
- 239000011686 zinc sulphate Substances 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims 2
- UUVBYOGFRMMMQL-UHFFFAOYSA-N calcium;phosphoric acid Chemical compound [Ca].OP(O)(O)=O UUVBYOGFRMMMQL-UHFFFAOYSA-N 0.000 claims 1
- 230000003760 hair shine Effects 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 229910001948 sodium oxide Inorganic materials 0.000 claims 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 10
- 239000011777 magnesium Substances 0.000 abstract description 10
- 229910052749 magnesium Inorganic materials 0.000 abstract description 9
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 229910000861 Mg alloy Inorganic materials 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 230000000399 orthopedic effect Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 210000000988 bone and bone Anatomy 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011173 biocomposite Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 210000000963 osteoblast Anatomy 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000002980 postoperative effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229940083608 sodium hydroxide Drugs 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 230000017423 tissue regeneration Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F3/1103—Making porous workpieces or articles with particular physical characteristics
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F3/1103—Making porous workpieces or articles with particular physical characteristics
- B22F3/1118—Making porous workpieces or articles with particular physical characteristics comprising internal reinforcements
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Mechanical Engineering (AREA)
- Engineering & Computer Science (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Dermatology (AREA)
- Transplantation (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicinal Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Materials For Medical Uses (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to a kind of preparation methods of magnesium-base porous compound material, the drawbacks of mechanical property can not ensure in too fast, degradation process for porous magnesium and magnesium alloy degradation rate, use β calcium phosphate phases and magnesium zinc zirconium for raw material, using sodium chloride crystal as pore creating material, by powder processed, dispensing, magnesium-base porous compound material block is made in vacuum plasma discharge sintering, this preparation method technique is advanced, data are accurately full and accurate, and the magnesium-base porous compound material of preparation is block, density 1.02g/cm3, porosity reaches 60%, and aperture≤450 μm, elasticity modulus 35GPa meets skeleton performance parameter, can meet clinical medical orthopedic implanting material and use, be the preparation method of advanced magnesium-base porous compound material.
Description
Technical field
The present invention relates to a kind of preparation methods of magnesium-base porous compound material, belong to magnesium-base porous biomaterial and prepare and answer
Technical field.
Background technology
Magnesium and magnesium alloy have good mechanical property, biocompatibility and degradability, become most potential biology
Material, porous structure can make bone tissue by pore development, be conducive to adherency, increment and differentiation of the osteoblast on its surface, promote
Bone tissue regeneration can accelerate the postoperative rehabilitation of patient；But degradation rate of the porous magnesium in human body is too fast, while hole
It is reduced in the presence of will also result in mechanical property, therefore porous magnesium and alloy are limited in clinical application by very much.
It is above-mentioned in order to solve the problems, such as, it can be combined with β calcium phosphate phases with magnesium zinc zircaloy, mechanical property and resistance to
Corrosive nature will be improved, and β calcium phosphate phases have good bioactivity, biocompatibility and bone guided effect, can
Overcome the disadvantage that degradation rate is too fast, the zinc-plated connection for enhancing metal and ceramic powders of β calcium phosphate phase powder surface chemistries；Together
When magnesium zinc zircaloy due to alloying element exist, corrosion resistance and mechanical property can be also improved.
Currently, the method for preparing porous magnesium-based Biocomposite material has vacuum seepage casting, powder metallurgic method, laser to beat
Kong Fa, but these methods all have that complex process, stability are poor, hole body structure control difficulty.
Invention content
Goal of the invention
The purpose of the present invention is the present situations and deficiency for background technology, are original with β calcium phosphate phases and magnesium zinc zircaloy powder
Material by powder processed, powder pre-treating, is matched powder, mixed powder, vacuum plasma discharge sintering, is made using sodium chloride crystal as pore creating material
Magnesium-base porous compound material, to improve the mechanical property and corrosion resistance of magnesium-based composite material.
Technical solution
The chemical substance material that the present invention uses is：Magnesium zinc zircaloy powder, β calcium phosphate phases, sodium chloride crystal, glycerine,
Absolute ethyl alcohol, sodium hydroxide, zinc sulfate, tartaric acid, ethylenediamine tetra-acetic acid, hydrazine, sodium acetate, deionized water, argon gas, graphite
Paper, it is as follows that a combination thereof prepares dosage：With gram, milliliter, millimeter, centimetre3For measurement unit
Magnesium zinc zircaloy powder：MgZnZr 15g ± 0.001g purity 99.98%
β calcium phosphate phases：β-Ca3(PO4)26g ± 0.001g purity 99.9%
Sodium chloride crystal：NaCl 9g ± 0.001g purity 99%
Sodium hydroxide：NaOH 2g ± 0.001g purity 99.9%
Glycerine：C3H8O3500mL ± 10mL purity 99%
Absolute ethyl alcohol：C2H6O 500mL ± 10mL purity 99.7%
Zinc sulfate：ZnSO4100g ± 0.001g purity 99%
Tartaric acid：C4H6O615g ± 0.001g purity 99%
Ethylenediamine tetra-acetic acid：C10H16N2O80.05g ± 0.001g purity 99%
Hydrazine：N2H4200mL ± 0.001mL purity 99%
Sodium acetate：C2H3NaO250g ± 0.001g purity 99%
Deionized water：H2O 3000mL ± 10mL purity 99%
Argon gas：Ar 800000cm3±100cm3Purity 99.99%
Graphite paper：Φ 60mm × 1mm, 2；
Preparation method is as follows：
(1) β calcium phosphate phases are pre-processed
1. configuring sodium hydrate aqueous solution
Sodium hydroxide 2g ± 0.001g sodium hydroxides are weighed, deionized water 500mL ± 0.001mL is measured, is placed in beaker,
5min is stirred, at the sodium hydrate aqueous solution of 0.1mol/L, PH=13；
2. impregnating calcium phosphate
β calcium phosphate phase 6g ± 0.001g are weighed, sodium hydrate aqueous solution 100mL ± 0.001mL is measured, are added in beaker,
30min is impregnated, at mixed liquor；
3. ultrasonic disperse
The beaker for filling mixed liquor is placed in ultrasonic disperser, ultrasonic disperse is carried out, ultrasonic frequency 40kHz surpasses
Sound jitter time 20min；
4. filtering, washing
Mixed liquor after ultrasonic disperse is placed in the Buchner funnel of bottle,suction, is filtered with miillpore filter, filter is retained
Cake discards filtrate；
Filter cake is placed in beaker, deionized water 200mL, agitator treating 10min, at mixed liquor is added；
Then it is filtered with miillpore filter, retains filter cake, discard cleaning solution；
5. being dried in vacuo
Filter cake is placed in silica dish, is put into vacuum drying chamber and is dried, 120 DEG C, vacuum degree 2Pa of drying temperature,
Drying time 300min, at β calcium phosphate phase powder granules；
(2) β calcium phosphate phases powder granule surface is zinc-plated
1. configuring galvanizing solution
Zinc sulfate 100g ± 0.001g, tartaric acid 15g ± 0.001g, ethylenediamine tetra-acetic acid 0.05g ± 0.001g are weighed, is measured
Ionized water 500mL ± 0.001mL is removed, is added in beaker, 5min is stirred, at zinc sulfate mixed solution；
Sodium acetate 50g ± 0.001g is weighed, hydrazine 200mL ± 0.001mL, deionized water 500mL ± 0.001mL are measured,
It is added in another beaker, 5min is stirred, at sodium acetate mixed solution, acid-base value PH=5；
2. preparing acid composite solution, ultrasonic disperse
Zinc sulfate mixed solution, sodium acetate mixed solution are placed in another beaker, are stirred, at acid compound molten
Liquid；
The beaker for filling acid composite solution is placed on ultrasonic disperser, ultrasonic disperse, ultrasonic frequency are carried out
40kHz, jitter time 20min；
3. pretreated β calcium phosphate phases powder granule 6g ± 0.001g is added in acid composite solution, continue to surpass
Sound disperses, ultrasonic frequency 40kHz, ultrasonic disperse time 20min, at zinc-plated mixed liquor；
Open the heating device of ultrasonic disperser, 80 DEG C of heating temperature, heating time 30min；
It is zinc-plated that surface is carried out in heating process；
DC power supply is passed through in zinc-plated mixed liquor, current strength 2A makes zinc-plated homogenization；
4. filtering；Zinc-plated mixed liquor is placed in the Buchner funnel of bottle,suction, is filtered with miillpore filter, filter is preserved
Cake discards filtrate；
5. washing filters；Filter cake is put into beaker, deionized water 200mL is added, stirs 10min；Then it is filtered with micropore
Film is filtered；Washing, which filters, to be repeated three times；
6. being dried in vacuo；Filter cake is put in silica dish, is subsequently placed in vacuum drying chamber, vacuum degree 2Pa, drying temperature
120 DEG C, drying time 300min, at zinc-plated β calcium phosphate phases powder granule；
(3) match powder
Weigh magnesium zinc zircaloy powder 15g ± 0.001g, zinc-plated β calcium phosphate phases powder 6g ± 0.001g, sodium chloride crystal 9g ±
0.001g is added in ball grinder, at mixed powder；
Magnesium zinc zircaloy powder：Zinc-plated β calcium phosphate phases powder：Sodium chloride crystal=5:2:3；
(4) ball milling, mixed powder
It is added agate ball into ball grinder, the volume ratio of agate ball and mixed powder is 6：1, ball milling revolution 300r/min, ball
Consume time 60min, at zinc-plated β calcium phosphate phases powder+magnesium zinc zirconium mixed powder after ball milling；
(5) molding, die-filling
1. molding, retractable die is manufactured with graphite material, and mold cavity is cylindrical shape, and mold cavity surface roughness is
Ra0.08-0.16μm；
2. it is die-filling, open-close type graphite jig is vertically arranged on steel tablet, and is fixed by fixed seat；
Graphite cushion block is put in mold cavity bottom, graphite paper is put on graphite cushion block top, puts and plate on graphite paper top
Zinc β calcium phosphate phases powder+magnesium zinc zirconium mixed powder puts graphite paper, in stone on zinc-plated β calcium phosphate phases powder+magnesium zinc zirconium mixed powder top
Put graphite briquetting in black paper top；
(6) vacuum-sintering
1. opening the outer water circulating cooling pipe of vacuum sintering furnace, outer water circulating cooling is carried out；
2. opening vacuum sintering furnace, die-filling graphite jig parallel vertical is moved on the workbench in vacuum sintering furnace,
It is closed；
3. opening the vacuum pump of vacuum sintering furnace, furnace air is extracted, pressure in furnace chamber is made to reach 2Pa；
4. opening argon bottle, argon gas, argon gas input speed 100cm are inputted into furnace chamber3/ min makes invariablenes pressure of liquid in furnace chamber
In 1 atmospheric pressure；
5. opening plasma discharge heater, 500 DEG C ± 1 DEG C of heating temperature, and constant temperature；Opening pressure motor, pressure electricity
Machine pressure 30MPa, constant temperature pressing time 5min, then stop heating, pressurization, and mold cools to 25 DEG C with the furnace；
6. vacuum sintering furnace is opened in blow-on, die sinking, retractable die is taken out, opens mold, takes out β calcium phosphate phases+magnesium zinc
Zirconium block, i.e. magnesium-base porous compound material；
(7) it polishes
With sand paper polishing β calcium phosphate phases+magnesium zinc zirconium block, block surface and periphery is made to clean；Block is cleaned with absolute ethyl alcohol
Body surface face and periphery keep block surface clean；
(8) pore creating material is removed
Clean block is placed in beaker, the sodium hydrate aqueous solution 500mL of 0.1mol/L is added, is impregnated at 25 DEG C
240min is used in combination magnetic stirrer, the dissolving of pore creating material sodium chloride crystal then to dry；
(9) it cleans
The block impregnated after drying is placed in beaker, absolute ethyl alcohol 300mL, soaking and washing 30min is added；
(10) it is dried in vacuo
Block is put in vacuum drying chamber to dry, 80 DEG C, vacuum degree 2Pa of drying temperature, drying time after soaking and washing
240min；
Magnesium-base porous compound material is obtained after drying；
(11) test, analysis and characterization
The pattern of the magnesium-base porous compound material of preparation, color and luster, mechanical property, density, metallographic structure, hole are examined
It surveys, analysis, characterize；
Metallographic structure and hole situation are detected with scanning electron microscope；
Porous material density is detected with Archimedes method；
Constituent content analysis is carried out with energy depressive spectroscopy；
Elasticity modulus analysis is carried out with tensile sample machine and foil gauge；
Conclusion：Magnesium-base porous compound material is cylindrical block, density 1.02g/cm3, porosity reaches 60%, hole
Diameter≤450 μm, elasticity modulus 35GPa；
(12) it packs, store
The magnesium-base porous compound material block of preparation is vacuum-packed with soft material, is stored in shady and cool clean environment, to be prevented
Damp, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.
Advantageous effect
There is apparent advance compared with the background technology, the present invention, be for mechanical property in magnesium and magnesium alloy degradation process
It the drawbacks of capable of can not ensureing, uses β calcium phosphate phases and magnesium zinc zirconium for matrix material, using sodium chloride crystal as pore creating material, passes through system
Powder, dispensing, vacuum plasma discharge sintering, are made magnesium-base porous compound material, and pore creating material, this preparation side are removed with alkaline solution
Method technique is advanced, and data are accurately full and accurate, and magnesium-base porous compound material is cylindrical block, density 1.02g/cm3, porosity
Up to 60%, aperture≤450 μm, elasticity modulus 35GPa meets skeleton performance parameter, is that advanced preparation magnesium-based is compound
The method of material.
Description of the drawings
Fig. 1 magnesium-base porous compound material vacuum-sintering state diagrams
Fig. 2 magnesium-base porous compound material cross-sectional morphology figures
Fig. 3 magnesium-base porous compound material X-ray diffraction intensity collection of illustrative plates
As shown in the figure, list of numerals is as follows：
Vacuum sintering furnace, 2, footstock, 3, pedestal, 4, bearing, 5, outer water circulating cooling pipe, 6, vacuum pump, 7, vacuum tube, 8,
Cooling water tank, 9, water pump, 10, outlet pipe, 11, return pipe, 12, workbench, 13, seaming chuck, 14, graphite jig, 15, graphite pads
Block, the 16, first graphite paper, 17, β calcium phosphate phases powder+magnesium zinc zirconium mixed powder, the 18, second graphite paper, 19, graphite briquetting, 20, go out
Tracheae valve, 21, pressure motor, 22, argon bottle, 23, argon gas valve, 24, tunger tube, 25, argon gas, 26, electric cabinet, 27, display screen,
28, indicator light, 29, power switch, 30, plasma discharge heating controller, 31, pressure electric machine controller, 32, vacuum pump control
Device, 33, water pump controller, the 34, first conducting wire, the 35, second conducting wire, 36, privates, 37, privates, 38, fixed seat,
39, furnace chamber, 40, plasma discharge heater.
Specific implementation mode
Below in conjunction with attached drawing, the present invention will be further described：
It is magnesium-base porous compound material vacuum-sintering state diagram, each portion position, connection relation are correct, by it shown in Fig. 1
Proportioning, sequentially operates.
The magnitude for preparing the chemical substance used is determined by pre-set range, with gram, milliliter, centimetre3For meter
Measure unit.
The sintering of magnesium-base porous compound material carries out in vacuum sintering furnace, is in argon gas protection, plasma discharge
It is completed in heating process；
Vacuum sintering furnace is vertical, and 1 lower part of vacuum sintering furnace is pedestal 3, top is footstock 2, and inside is furnace chamber 39；The bottom of at
3 tops of seat are equipped with holder 4, and vacuum pump 6, water tank 8 are equipped in holder 4；6 top of vacuum pump is equipped with vacuum tube 7, on vacuum tube 7
Portion stretches into furnace chamber 39；8 top of water tank is equipped with water pump 9, and 9 top of water pump connects outlet pipe 10, and outlet pipe 10 connects outer water cycle
Cooling tube 5, outer water circulating cooling pipe 5 connect return pipe 11, and return pipe 11 connects water tank 8, forms outer water circulating cooling；In furnace chamber
Bottom is equipped with workbench 12 in 39, and portion is disposed vertically graphite jig 14 on table 12, and is fixed by firm banking 38, in stone
Bottom is graphite cushion block 15 in black mold 14, is the first graphite paper 16 on 15 top of graphite cushion block, on 16 top of the first graphite paper
For β calcium phosphate phases powder+magnesium zinc zirconium mixed powder 17, β calcium phosphate phases powder+17 top of magnesium zinc zirconium mixed powder is the second graphite paper 18, the
Two graphite papers, 18 top is graphite briquetting 19, and 19 top of graphite briquetting connects seaming chuck 13, and 13 top of seaming chuck connects footstock 2,
And connect pressure motor 21；Plasma discharge heater 30 is equipped on the inner wall of vacuum sintering furnace 1；In vacuum sintering furnace 1
Upper right quarter is equipped with outlet pipe valve 20；The left part of vacuum sintering furnace 1 be equipped with argon bottle 22,22 top of argon bottle be equipped with argon gas valve 23,
Tunger tube 24, and argon gas 25 is inputted into furnace chamber 39；It is equipped with electric cabinet 26 in the right part of vacuum sintering furnace 1, on electric cabinet 26
Equipped with display screen 27, indicator light 28, power switch 29, plasma discharge heating controller 30, pressure electric machine controller 31, vacuum
Pump controller 32, water pump controller 33；Electric cabinet 26 connects water pump 9 by the first conducting wire 34, is connected very by the second conducting wire 35
Sky pump 6 connects plasma discharge heater 40 by privates 36, connects pressure motor 21 by privates.
It is magnesium-base porous compound material cross section shape appearance figure shown in Fig. 2, as shown in the figure, scanning electron microscope is amplified to be seen under 50 times
Examine pore size, porosity is up to 60%, aperture≤450 μm.
It is magnesium-base porous compound material energy spectrum analysis collection of illustrative plates, as shown in the figure, ordinate is diffracted intensity, horizontal seat shown in Fig. 3
It is designated as the angle of diffraction；Content of magnesium is 70.5% in magnesium-base porous compound material, oxygen content 17.8%, sodium content 3.7%, zinc contain
Amount is 2.5%, chlorinity 2.4%, calcium content 1.1%, phosphorus content 1.0%, zirconium content 1.0%, and magnesium is located at 1 ° 30 '
For top.
Claims (2)
1. a kind of preparation method of magnesium-base porous compound material, it is characterised in that
The chemical substance material used is：Magnesium zinc zircaloy powder, β calcium phosphate phases, sodium chloride crystal, glycerine, absolute ethyl alcohol, hydrogen
Sodium oxide molybdena, zinc sulfate, tartaric acid, ethylenediamine tetra-acetic acid, hydrazine, sodium acetate, deionized water, argon gas, graphite paper, a combination thereof prepare
Dosage is as follows：With gram, milliliter, millimeter, centimetre3For measurement unit
Magnesium zinc zircaloy powder：MgZnZr 15g ± 0.001g purity 99.98%
β calcium phosphate phases：β-Ca3(PO4)26g ± 0.001g purity 99.9%
Sodium chloride crystal：NaCl 9g ± 0.001g purity 99%
Sodium hydroxide：NaOH 2g ± 0.001g purity 99.9%
Glycerine：C3H8O3500mL ± 10mL purity 99%
Absolute ethyl alcohol：C2H6O 500mL ± 10mL purity 99.7%
Zinc sulfate：ZnSO4100g ± 0.001g purity 99%
Tartaric acid：C4H6O615g ± 0.001g purity 99%
Ethylenediamine tetra-acetic acid：C10H16N2O80.05g ± 0.001g purity 99%
Hydrazine：N2H4200mL ± 0.001mL purity 99%
Sodium acetate：C2H3NaO250g ± 0.001g purity 99%
Deionized water：H2O 3000mL ± 10mL purity 99%
Argon gas：Ar 800000cm3±100cm3Purity 99.99%
Graphite paper：Φ 60mm × 1mm, 2；
Preparation method is as follows：
(1) β calcium phosphate phases are pre-processed
1. configuring sodium hydrate aqueous solution
Sodium hydroxide 2g ± 0.001g sodium hydroxides are weighed, deionized water 500mL ± 0.001mL is measured, is placed in beaker, are stirred
5min, at the sodium hydrate aqueous solution of 0.1mol/L, PH=13；
2. impregnating calcium phosphate
β calcium phosphate phase 6g ± 0.001g are weighed, sodium hydrate aqueous solution 100mL ± 0.001mL is measured, are added in beaker, are impregnated
30min, at mixed liquor；
3. ultrasonic disperse
The beaker for filling mixed liquor is placed in ultrasonic disperser, ultrasonic disperse, ultrasonic frequency 40kHz, ultrasound point are carried out
Dissipate time 20min；
4. filtering, washing
Mixed liquor after ultrasonic disperse is placed in the Buchner funnel of bottle,suction, is filtered with miillpore filter, filter cake is retained, abandons
Go filtrate；
Filter cake is placed in beaker, deionized water 200mL, agitator treating 10min, at mixed liquor is added；
Then it is filtered with miillpore filter, retains filter cake, discard cleaning solution；
5. being dried in vacuo
Filter cake is placed in silica dish, is put into vacuum drying chamber and is dried, 120 DEG C, vacuum degree 2Pa of drying temperature is dry
Time 300min, at β calcium phosphate phase powder granules；
(2) β calcium phosphate phases powder granule surface is zinc-plated
1. configuring galvanizing solution
Zinc sulfate 100g ± 0.001g, tartaric acid 15g ± 0.001g, ethylenediamine tetra-acetic acid 0.05g ± 0.001g are weighed, measurement is gone
Ionized water 500mL ± 0.001mL is added in beaker, 5min is stirred, at zinc sulfate mixed solution；
Sodium acetate 50g ± 0.001g is weighed, hydrazine 200mL ± 0.001mL, deionized water 500mL ± 0.001mL are measured, is added
In another beaker, 5min is stirred, at sodium acetate mixed solution, acid-base value PH=5；
2. preparing acid composite solution, ultrasonic disperse
Zinc sulfate mixed solution, sodium acetate mixed solution are placed in another beaker, are stirred, at acid composite solution；
The beaker for filling acid composite solution is placed on ultrasonic disperser, progress ultrasonic disperse, ultrasonic frequency 40kHz,
Jitter time 20min；
3. pretreated β calcium phosphate phases powder granule 6g ± 0.001g is added in acid composite solution, continue ultrasound point
It dissipates, ultrasonic frequency 40kHz, ultrasonic disperse time 20min, at zinc-plated mixed liquor；
Open the heating device of ultrasonic disperser, 80 DEG C of heating temperature, heating time 30min；
It is zinc-plated that surface is carried out in heating process；
DC power supply is passed through in zinc-plated mixed liquor, current strength 2A makes zinc-plated homogenization；
4. filtering；Zinc-plated mixed liquor is placed in the Buchner funnel of bottle,suction, is filtered with miillpore filter, filter cake is preserved, abandons
Go filtrate；
5. washing filters；Filter cake is put into beaker, deionized water 200mL is added, stirs 10min；Then use miillpore filter into
Row filters；Washing, which filters, to be repeated three times；
6. being dried in vacuo；Filter cake is put in silica dish, is subsequently placed in vacuum drying chamber, vacuum degree 2Pa, drying temperature 120
DEG C, drying time 300min, at zinc-plated β calcium phosphate phases powder granule；
(3) match powder
Weigh magnesium zinc zircaloy powder 15g ± 0.001g, zinc-plated β calcium phosphate phases powder 6g ± 0.001g, sodium chloride crystal 9g ±
0.001g is added in ball grinder, at mixed powder；
Magnesium zinc zircaloy powder：Zinc-plated β calcium phosphate phases powder：Sodium chloride crystal=5:2:3；
(4) ball milling, mixed powder
It is added agate ball into ball grinder, the volume ratio of agate ball and mixed powder is 6：1, ball milling revolution 300r/min, when ball milling
Between 60min, at zinc-plated β calcium phosphate phases powder+magnesium zinc zirconium mixed powder after ball milling；
(5) molding, die-filling
1. molding, retractable die is manufactured with graphite material, and mold cavity is cylindrical shape, and mold cavity surface roughness is Ra0.08-
0.16μm；
2. it is die-filling, open-close type graphite jig is vertically arranged on steel tablet, and is fixed by fixed seat；
Graphite cushion block is put in mold cavity bottom, graphite paper is put on graphite cushion block top, zinc-plated β phases are put on graphite paper top
Phosphoric acid calcium powder+magnesium zinc zirconium mixed powder puts graphite paper, on graphite paper on zinc-plated β calcium phosphate phases powder+magnesium zinc zirconium mixed powder top
Put graphite briquetting in portion；
(6) vacuum-sintering
1. opening the outer water circulating cooling pipe of vacuum sintering furnace, outer water circulating cooling is carried out；
2. opening vacuum sintering furnace, die-filling graphite jig parallel vertical is moved on the workbench in vacuum sintering furnace, it is closed；
3. opening the vacuum pump of vacuum sintering furnace, furnace air is extracted, pressure in furnace chamber is made to reach 2Pa；
4. opening argon bottle, argon gas, argon gas input speed 100cm are inputted into furnace chamber3/ min makes in furnace chamber invariablenes pressure of liquid at 1
Atmospheric pressure；
5. opening plasma discharge heater, 500 DEG C ± 1 DEG C of heating temperature, and constant temperature；Opening pressure motor, pressure motor pressure
Strong 30MPa, constant temperature pressing time 5min, then stop heating, pressurization, and mold cools to 25 DEG C with the furnace；
6. vacuum sintering furnace is opened in blow-on, die sinking, retractable die is taken out, opens mold, takes out β calcium phosphate phases+magnesium zinc zirconium block
Body, i.e. magnesium-base porous compound material；
(7) it polishes
With sand paper polishing β calcium phosphate phases+magnesium zinc zirconium block, block surface and periphery is made to clean；Block table is cleaned with absolute ethyl alcohol
Face and periphery keep block surface clean；
(8) pore creating material is removed
Clean block is placed in beaker, the sodium hydrate aqueous solution 500mL of 0.1mol/L is added, is impregnated at 25 DEG C
240min is used in combination magnetic stirrer, the dissolving of pore creating material sodium chloride crystal then to dry；
(9) it cleans
The block impregnated after drying is placed in beaker, absolute ethyl alcohol 300mL, soaking and washing 30min is added；
(10) it is dried in vacuo
Block is put in vacuum drying chamber to dry, 80 DEG C, vacuum degree 2Pa of drying temperature, drying time after soaking and washing
240min；
Magnesium-base porous compound material is obtained after drying；
(11) test, analysis and characterization
The pattern of the magnesium-base porous compound material of preparation, color and luster, mechanical property, density, metallographic structure, hole are detected,
Analysis, characterization；
Metallographic structure and hole situation are detected with scanning electron microscope；
Porous material density is detected with Archimedes method；
Constituent content analysis is carried out with energy depressive spectroscopy；
Elasticity modulus analysis is carried out with tensile sample machine and foil gauge；
Conclusion：Magnesium-base porous compound material is cylindrical block, density 1.02g/cm3, porosity reaches 60%, and aperture≤
450 μm, elasticity modulus 35GPa；
(12) it packs, store
The magnesium-base porous compound material block of preparation is vacuum-packed with soft material, is stored in shady and cool clean environment, moisture-proof, anti-
It shines, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.
2. according to a kind of preparation method of magnesium-base porous compound material described in claim 1, it is characterised in that：
The sintering of magnesium-base porous compound material carries out in vacuum sintering furnace, is in argon gas protection, plasma discharge heating
It completes in the process；
Vacuum sintering furnace is vertical, and vacuum sintering furnace (1) lower part is pedestal (3), top is footstock (2), and inside is furnace chamber (39)；
It is equipped with holder (4) on pedestal (3) top, vacuum pump (6), water tank (8) are equipped in holder (4)；Vacuum pump (6) top is equipped with true
Blank pipe (7), vacuum tube (7) top are stretched into furnace chamber (39)；Water tank (8) top is equipped with water pump (9), and water pump (9) top connects out
Water pipe (10), outlet pipe (10) connect outer water circulating cooling pipe (5), outer water circulating cooling pipe (5) connection return pipe (11), return water
(11) connection water tank (8) is managed, outer water circulating cooling is formed；It is equipped with workbench (12) in furnace chamber (39) interior bottom, in workbench
(12) upper vertical places graphite jig (14), and fixed by firm banking (38), is graphite in graphite jig (14) interior bottom
Cushion block (15) is the first graphite paper (16) on graphite cushion block (15) top, is β calcium phosphate phase powder on the first graphite paper (16) top
+ magnesium zinc zirconium mixed powder (17), β calcium phosphate phases powder+magnesium zinc zirconium mixed powder (17) top are the second graphite paper (18), the second graphite paper
(18) top is graphite briquetting (19), and graphite briquetting (19) top connects seaming chuck (13), and seaming chuck (13) top connects footstock
(2), and pressure motor (21) is connected；Plasma discharge heater (30) is equipped on the inner wall of vacuum sintering furnace (1)；In vacuum
The upper right quarter of sintering furnace (1) is equipped with outlet pipe valve (20)；The left part of vacuum sintering furnace (1) is equipped with argon bottle (22), argon bottle
(22) top is equipped with argon gas valve (23), tunger tube (24), and the input argon gas (25) into furnace chamber (39)；In vacuum sintering furnace (1)
Right part be equipped with electric cabinet (26), on electric cabinet (26) be equipped with display screen (27), indicator light (28), power switch (29), etc.
Ionic discharge heating controller (30), pressure electric machine controller (31), controller for vacuum pump (32), water pump controller (33)；Electricity
Control case (26) connects water pump (9) by the first conducting wire (34), connects vacuum pump (6) by the second conducting wire (35), led by third
Line (36) connects plasma discharge heater (40), connects pressure motor (21) by privates.
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| CN107400837B (en) * | 2017-07-31 | 2018-08-21 | 太原理工大学 | A kind of preparation method of nickle-based block non-crystaline amorphous metal |
| CN107855528B (en) * | 2017-10-31 | 2019-10-08 | 太原理工大学 | A kind of preparation method of porous zinc magnesium alloy/hydroxyapatite composite material |
| CN108788159A (en) * | 2018-07-17 | 2018-11-13 | 太原理工大学 | A kind of ultrasonic wave auxiliary hot-pressed sintering furnace |
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