CN106834774A - A kind of novel dental niobium silver alloy and preparation method thereof - Google Patents
A kind of novel dental niobium silver alloy and preparation method thereof Download PDFInfo
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- CN106834774A CN106834774A CN201710086861.XA CN201710086861A CN106834774A CN 106834774 A CN106834774 A CN 106834774A CN 201710086861 A CN201710086861 A CN 201710086861A CN 106834774 A CN106834774 A CN 106834774A
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- LUPQXSQTQUHAKA-UHFFFAOYSA-N [Nb].[Ag] Chemical compound [Nb].[Ag] LUPQXSQTQUHAKA-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910001316 Ag alloy Inorganic materials 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 66
- 239000000956 alloy Substances 0.000 claims abstract description 47
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 42
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 20
- 239000010955 niobium Substances 0.000 claims abstract description 12
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 10
- 239000006104 solid solution Substances 0.000 claims abstract description 7
- 239000011812 mixed powder Substances 0.000 claims description 35
- 239000000843 powder Substances 0.000 claims description 33
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 30
- 238000000137 annealing Methods 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 23
- 239000007789 gas Substances 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 13
- 239000011261 inert gas Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000001307 helium Substances 0.000 claims description 10
- 229910052734 helium Inorganic materials 0.000 claims description 10
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 7
- 239000005548 dental material Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 abstract description 13
- 230000007797 corrosion Effects 0.000 abstract description 12
- 238000005260 corrosion Methods 0.000 abstract description 12
- 238000002156 mixing Methods 0.000 abstract description 7
- 229910052709 silver Inorganic materials 0.000 abstract description 7
- 239000004332 silver Substances 0.000 abstract description 7
- 239000002932 luster Substances 0.000 abstract description 6
- 230000003115 biocidal effect Effects 0.000 abstract description 5
- 239000003564 dental alloy Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000009413 insulation Methods 0.000 description 11
- 238000010792 warming Methods 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910002804 graphite Inorganic materials 0.000 description 8
- 239000010439 graphite Substances 0.000 description 8
- 238000000227 grinding Methods 0.000 description 8
- 230000000845 anti-microbial effect Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 201000010099 disease Diseases 0.000 description 3
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 239000002707 nanocrystalline material Substances 0.000 description 3
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000003701 mechanical milling Methods 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000497 Amalgam Inorganic materials 0.000 description 1
- 239000000120 Artificial Saliva Substances 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 208000010641 Tooth disease Diseases 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000004053 dental implant Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000018984 mastication Effects 0.000 description 1
- 238000010077 mastication Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 230000003239 periodontal effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 229910001256 stainless steel alloy Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/84—Preparations for artificial teeth, for filling teeth or for capping teeth comprising metals or alloys
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Thermal Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The present invention relates to a kind of novel dental niobium silver alloy and preparation method thereof, the niobium silver alloy is made up of by molar content 60 99.95% niobium and 0.05 40% silver.High-energy ball milling is carried out in high energy ball mill after under an inert atmosphere mixing silver powder and niobium powder, it is forced miscible formation single phase solid solution, then sinter block niobium silver two-phase alloys material into using discharge plasma sintering technology.The niobium silver alloy is made up of the niobium crystal grain and silver-colored crystal grain of nanoscale, crystallite dimension is 20 300nm, with excellent biocompatibility and antibiotic property, its compressive strength is up to 1.0 1.8GPa, Vickers hardness is up to 3.0 6.5GPa, while there is good corrosion resistance and wearability, and surface is presented metallic luster, it is a kind of new dental alloy, has a good application prospect.
Description
Technical field
Prepared the present invention relates to alloy and dental material preparation field, and in particular to a kind of novel dental niobium silver alloy
Material and preparation method thereof
Background technology
Dental disorder is one of most common disease of human society, including tooth defect, periodontal missing etc..Treatment dentistry disease
The general method of disease is using dental implant reparation.Material currently used for oral restoration mainly includes alloy, ceramics and tree
Fat three major types.Wherein alloy repair materials are due to intensity very high, hardness, toughness and wear-resistant and be used widely.
Existing dental alloy material category is various.Such as Ni substrate alloy, stainless steel, titanium alloy and silver amalgam.
Due to oral environment it is complicated, acid-base property fluctuation is big, it is desirable to which alloy material possesses good corrosion resistance.While mastication processes
Tooth is engaged stress, it is necessary to alloy material possesses intensity higher, hardness and wearability.In addition, oral environment connects with the external world
Touch frequent, easy breed bacteria is, it is necessary to alloy material possesses good anti-microbial property.And due to alloy material and tissue
Directly contact is, it is necessary to it has good biocompatibility, it is impossible to produce side effect to human body cell.It is existing with reference to above-mentioned requirements
Some alloy materials are difficult to be provided simultaneously with above advantage, and such as nickel alloy has toxicity clinical in cell due to nickel ion
Abandon using, stainless steel and titanium alloy are fine in terms of structural strength and wearability, but cannot meet the requirement of antibacterial.Therefore grind
Make corrosion-resistant, wear-resistant, intensity high, and be dental material development with the material of good biocompatibility and antibiotic property
New direction.
The content of the invention
For the deficiencies in the prior art, the present invention provides a kind of novel dental niobium silver alloy.The alloy
Material is combined and is prepared by high-energy ball milling machinery alloying and discharge plasma sintering technology.Prepared block niobium
The crystallite dimension of silver alloy is 20-300nm, with excellent biocompatibility and hardness it is high, intensity is high, it is wear-resistant,
There is metallic luster, and good corrosion resistance and anti-microbial property is shown in oral environment, be a kind of new
Dental material.
To achieve the above object, the present invention selects following technical scheme：
In a first aspect, the present invention provides a kind of niobium silver alloy, the niobium silver alloy press molar content by
Following components is constituted：Niobium 60-99.95%, silver-colored 0.05-40%.
Niobium silver alloy prepared by the present invention is made up of the niobium crystal grain and silver-colored crystal grain of nanoscale, and crystallite dimension is 20-
300nm, with excellent biocompatibility and antibiotic property, up to 1.0-1.8GPa, Vickers hardness is up to 3.0- for its compressive strength
6.5GPa, while there is good corrosion resistance and wearability, and surface is presented metallic luster, is a kind of new dental alloy
Material.
In the present invention, based on molar content, the content of niobium is 60-99.95% in the niobium silver alloy, for example
Can be specific between 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95% or 99.5%, and above-mentioned numerical value
Point value, as space is limited and for concise consideration, the present invention specific point value that no longer scope described in exclusive list includes.
Corresponding, based on molar content, the content of silver is 0.05-40% in the niobium silver alloy, for example
Can be specific between 0.05%, 5%, 10%, 15%, 20%, 25%, 30%, 35% or 40%, and above-mentioned numerical value
Value, as space is limited and for concise consideration, the present invention specific point value that no longer scope described in exclusive list includes.
According to the present invention, the crystallite dimension of the niobium silver alloy is 20-300nm, for example can be 20nm, 50nm,
Specific point value between 100nm, 150nm, 200nm, 250nm or 300nm, and above-mentioned numerical value, as space is limited and for simplicity
Consideration, the present invention specific point value that no longer scope described in exclusive list includes.
Niobium silver alloy prepared by the present invention is nanocrystalline material, and its crystallite dimension is between 20-300nm.Crystal grain is thin
Change can greatly improve yield strength, hardness and the anti-wear performance of material.
According to the present invention, the compressive strength of the niobium silver alloy is 1.0-1.8GPa, for example can be 1.0GPa,
Tool between 1.1GPa, 1.2GPa, 1.3GPa, 1.4GPa, 1.5GPa, 1.6GPa, 1.7GPa or 1.8GPa, and above-mentioned numerical value
Body point value, as space is limited and for concise consideration, the present invention specific point value that no longer scope described in exclusive list includes.
According to the present invention, the Vickers hardness of the niobium silver alloy is 3.0-6.5GPa, for example can be 3.0GPa,
Specific point value between 3.5GPa, 4.0GPa, 4.5GPa, 5.0GPa, 5.5GPa, 6.0GPa or 6.5GPa, and above-mentioned numerical value,
As space is limited and for concise consideration, the present invention specific point value that no longer scope described in exclusive list includes.
Second aspect, the present invention provides a kind of preparation method of niobium silver alloy as described in relation to the first aspect, the side
Method is comprised the following steps：
(1) under an inert atmosphere, silver powder and niobium powder are mixed to get mixed-powder, height is then carried out in high energy ball mill
Energy ball milling, obtains niobium silver solid solution alloy powder；
(2) alloy powder that step (1) is obtained is carried out into discharge plasma sintering, furnace cooling after the completion of sintering is obtained
To block niobium silver alloy.
Because niobium silver point difference is huge, and two-phase is completely immiscible under equilibrium condition, and traditional method of smelting is difficult to smelt.
The present invention makes niobium silver force miscible formation single phase solid solution, in discharge plasma sintering process, silver-colored edge by high-energy ball milling
Niobium crystal boundary is separated out, so as to form nanocrystalline niobium silver two-phase alloys, is allowed to have niobium element excellent corrosion resistance and bio-compatible concurrently
Property and the excellent anti-microbial property of silver element.
Niobium silver powder is forced miscible formation single phase solid solution by the present invention by high-energy ball milling, and crystal grain refinement is arrived
Below 10nm, help to increase powder table/interface can, strain energy and specific surface area, so as to increase powder active so that sintering
When, combines more rapid, while the powder particle for refining reduces space between powder, cause high can be obtained at a lower temperature
Density.
According to the present invention, the purity of step (1) the niobium powder is more than 99%, for example can be 99%, 99.1%,
99.2%th, 99.3%, 99.3%, 99.4%, 99.5%, 99.6%, 99.7%, 99.8%, 99.9%, 99.99%,
Specific point value between 99.999% or 100%, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention is not
The specific point value that scope described in exclusive list includes again.
The purity of step (1) the niobium powder is preferably more than 99.99% in the present invention.
According to the present invention, the purity of step (1) described silver powder is more than 99%, for example can be 99%, 99.1%,
99.2%th, 99.3%, 99.3%, 99.4%, 99.5%, 99.6%, 99.7%, 99.8%, 99.9%, 99.99%,
Specific point value between 99.999% or 100%, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention is not
The specific point value that scope described in exclusive list includes again.And the specific point value between above-mentioned numerical value, as space is limited and for letter
Bright consideration, the present invention specific point value that no longer scope described in exclusive list includes.
The purity of step (1) described silver powder is preferably more than 99.99% in the present invention.
The purity of niobium powder and silver powder is higher, and gained niobium silver alloy purity is higher, and its performance is more excellent.
According to the present invention, abrading-ball and the mass ratio of mixed-powder are (4-10) in step (1) described Process During High Energy Ball Milling:1,
For example can be 4:1、5:1、6:1、7:1、8:1、9:1 or 10:Specific point value between 1, and above-mentioned numerical value, as space is limited and
For concise consideration, the present invention specific point value that no longer scope described in exclusive list includes.
When the mass ratio of abrading-ball and mixed-powder is excessive, can increase between abrasive body and between abrasive body and liner plate because
Impact friction and produce idle work to be lost, increase power consumption and ball consumption, yield reduction, and abrasive body constituent impurity can be increased contain
Amount；Then abrasive material is excessive in ball grinder when mass ratio is too small, and abrading-ball moves slow down in the powder, can also reduce milling efficiency, unfavorable
In crystal grain refinement.
Abrading-ball is preferably (4-8) with the mass ratio of mixed-powder in step (1) described mechanical milling process in the present invention:1, enter one
Step is preferably 5:1.
Preferred abrading-ball not only improves energy utilization efficiency with the mass ratio of mixed-powder, reduces abrasive body constituent impurity dense
Degree, moreover it is possible to obtain the powder of superfine nano-crystalline.
According to the present invention, the time of step (1) described high-energy ball milling is 1-50h, for example can be 1h, 5h, 10h, 15h,
Specific point value between 20h, 25h, 30h, 35h, 40h, 45h or 50h, and above-mentioned numerical value, as space is limited and for simplicity
Consider, the present invention specific point value that no longer scope described in exclusive list includes.
According to the present invention, step (1) described inert gas is helium and/or argon gas.Mechanical milling process enters under an inert gas
Row can avoid mixed-powder from being oxidized and introduce impurity.
According to the present invention, the rotational frequency of the fixture of step (1) described high energy ball mill is 15-20Hz, for example, can be
Specific point value between 15Hz, 16Hz, 17Hz, 18Hz, 19Hz or 20Hz, and above-mentioned numerical value, as space is limited and for simplicity
Consideration, the present invention specific point value that no longer scope described in exclusive list includes.
The rotational frequency of the fixture of step (1) described high energy ball mill is preferably 17Hz in the present invention.
According to the present invention, the rotating speed of step (1) described high energy ball mill is 1600-1800r/min, for example, can be
It is specific between 1600r/min, 1650r/min, 1700r/min, 1750r/min or 1800r/min, and above-mentioned numerical value
Value, as space is limited and for concise consideration, the present invention specific point value that no longer scope described in exclusive list includes.
The rotating speed of step (1) described high energy ball mill is preferably 1725r/min in the present invention.
In discharge plasma sintering process, discharge plasma is produced between powder particle, powder is be combined with each other.Put
Electro-plasma sintering can not only be such that silver is separated out along niobium crystal boundary, form nanocrystalline niobium silver two-phase alloys, and gained alloy structure is thin
It is small uniform.In conventional pressurized sintering process, crystal grain is grown up rapidly, it is impossible to obtain nanocrystalline material.
For more common sintering, discharge plasma sintering have homogeneous heating, programming rate is fast, sintering temperature is low,
The advantages of sintering time is short, production efficiency is high.The niobium silver alloy intensity and hardness obtained after discharge plasma sintering are obtained greatly
Width is improved, with good abrasion resistance properties.
According to the present invention, the temperature of step (2) the discharge plasma sintering is 800-950 DEG C, for example, can be 800
DEG C, the specific point value between 850 DEG C, 900 DEG C or 950 DEG C, and above-mentioned numerical value, as space is limited and for concise consideration, this
The specific point value that scope described in invention no longer exclusive list includes.
Sintering temperature is too high to make silver fusing segregation and skewness, the too low then material of temperature not easy-formation, consistency drop
It is low.
According to the present invention, the time of step (2) discharge plasma sintering is 1-30min, for example can be 1min,
Specific point value between 5min, 10min, 15min, 20min, 25min or 30min, and above-mentioned numerical value, as space is limited and for
Concise consideration, the present invention specific point value that no longer scope described in exclusive list includes.
Sintering time is long to make crystal grain grow up, it is impossible to obtain nanocrystalline material, the time is too short, material cannot be molded.
According to the present invention, the pressure of step (2) the discharge plasma sintering is 10-100MPa, for example, can be
10MPa, 20MPa, 30MPa, 40MPa, 50MPa, 60MPa, 70MPa, 80MPa, 90MPa or 100MPa, and above-mentioned numerical value it
Between specific point value, as space is limited and for concise consideration, it is specific that the present invention no longer scope described in exclusive list includes
Value.
Sintering pressure is too high to cause material internal residual stress high, reduce service life, and hypotony can then reduce block
Body material density.
Sintering of the present invention is carried out in discharge plasma sintering stove, to persistently adding in stove in sintering process
Pressure, unloading pressure immediately after terminating, it is to avoid generation residual stress.
According to the present invention, the heating rate of step (2) the discharge plasma sintering is 20-100 DEG C/min, for example may be used
Be 20 DEG C/min, 30 DEG C/min, 40 DEG C/min, 50 DEG C/min, 60 DEG C/min, 70 DEG C/min, 80 DEG C/min, 90 DEG C/min or
Specific point value between 100 DEG C/min, and above-mentioned numerical value, as space is limited and for concise consideration, no longer limit of the invention
Enumerate the specific point value that the scope includes.
Heating rate is too fast to make the reduction of alloy material consistency, can then increase sintering time slowly excessively, crystal grain is grown up, nothing
Method obtains nanometer crystal alloy.
Alternatively, the present invention makes annealing treatment to the block niobium silver alloy that step (2) is obtained, it is therefore an objective to which regulation and control are brilliant
Grain size, eliminates tissue defects and internal stress, while obtaining the niobium silver alloy of various grain sizes.
According to the present invention, the annealing is carried out in vacuum drying oven or the heat-treatment furnace of inert gas shielding；
According to the present invention, the temperature of the annealing is 400-800 DEG C, for example can be 400 DEG C, 450 DEG C, 500 DEG C,
Specific point value between 550 DEG C, 600 DEG C, 650 DEG C, 700 DEG C, 750 DEG C or 800 DEG C, and above-mentioned numerical value, as space is limited and goes out
In concise consideration, the present invention specific point value that no longer scope described in exclusive list includes.
According to the present invention, the time of the annealing is 0.5-3h, for example, can be 0.5h, 1h, 1.5h, 2h, 2.5h
Or the specific point value between 3h, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer exclusive list institute
State the specific point value that scope includes.
According to the present invention, the heating rate of the annealing is 5-50 DEG C/min, for example can be 5 DEG C/min, 10 DEG C/
Min, 15 DEG C/min, 20 DEG C/min, 25 DEG C/min, 30 DEG C/min, 35 DEG C/min, 40 DEG C/min, 45 DEG C/min or 50 DEG C/min,
And the specific point value between above-mentioned numerical value, as space is limited and for concise consideration, model no longer described in exclusive list of the invention
Enclose including specific point value.
According to the present invention, the inert gas used during the annealing is helium and/or argon gas.
Used as preferred technical scheme, the preparation method of niobium silver alloy of the present invention is comprised the following steps：
(1) under an inert atmosphere, silver powder and niobium powder are mixed to get mixed-powder, then the high energy ball in high energy ball mill
Mill 1-50h, obtains niobium silver solid solution alloy powder；Wherein, the purity of the silver powder and niobium powder is more than 99%, the high energy ball
Abrading-ball and the mass ratio of mixed-powder are (4-10) during mill:1, the inert gas is helium and/or argon gas, the high energy
The rotational frequency of the fixture of ball mill is 15-20Hz, and rotating speed is 1600-1800r/min；
(2) alloy powder that step (1) is obtained is carried out into discharge plasma sintering, block niobium silver is obtained after the completion of sintering
Alloy material；Wherein, the temperature of discharge plasma sintering is 800-950 DEG C, the discharge plasma sintering when
Between be 1-30min, the pressure of discharge plasma sintering is 10-100MPa, the intensification of the discharge plasma sintering
Speed is 20-100 DEG C/min；
(3) the block niobium silver alloy for obtaining step (2) is made annealing treatment；Wherein, the annealing is true
Carried out in empty stove or the heat-treatment furnace of inert gas shielding, the temperature of the annealing is 400-800 DEG C, the annealing
Time be 0.5-3h, the heating rate of the annealing is 5-50 DEG C/min, and the inert gas is helium and/or argon
Gas.
The third aspect, the present invention provides a kind of niobium silver alloy as described in relation to the first aspect answering as dental material
With.
Niobium silver alloy has metallic luster, surface-brightening after polishing, and its compressive strength reaches 1.0-1.8GPa, Vickers
Stiffness reaches 3.0-6.5GPa, and with good wear-resistant and decay resistance, and biocompatibility is excellent, is a kind of reason
The dental material thought.When in niobium silver alloy in oral environment, silver separates out silver ion prior to salivary component reaction, plays antibacterial
Effect, and niobium forms passivating film, corrosion resistance is strong.
Compared with prior art, the present invention at least has the advantages that：
(1) niobium silver alloy crystallite dimension prepared by the present invention is 20-300nm, with excellent biocompatibility and
Antibiotic property, up to 1.0-1.8GPa, Vickers hardness is up to 3.0-6.5GPa for its compressive strength, while having good corrosion resistance
And wearability, and surface is presented metallic luster, is a kind of new dental alloy, has a good application prospect.
(2) instant invention overcomes niobium silver point difference is huge and equilibrium condition under two-phase it is completely immiscible, traditional melting side
Method is difficult to the problem smelted, and sinters to be combined successfully to have prepared by high-energy ball milling machinery alloying and discharge plasma and receives
The brilliant niobium silver alloy of rice.
Brief description of the drawings
Fig. 1 is the outside drawing of niobium silver alloy prepared by the embodiment of the present invention 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of niobium silver alloy prepared by the embodiment of the present invention 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of niobium silver alloy prepared by the embodiment of the present invention 5.
Specific embodiment
Further illustrate technical scheme below in conjunction with the accompanying drawings and by specific embodiment.
For the present invention is better described, technical scheme is readily appreciated, it is of the invention typical but non-limiting
Embodiment is as follows：
Embodiment 1
(1) in the glove box protected full of argon gas, by mole meter, the niobium powder of 20% silver powder and 80% is entered
Row mixing, obtains mixed-powder, and the purity of niobium powder and silver powder is 99.99%；Mixed-powder is placed in high energy ball mill, is controlled
Abrading-ball processed is 5 with the mass ratio of mixed-powder:1, high-energy ball milling 12h, obtain alloy powder；
(2) alloy powder that step (1) is obtained is placed in graphite grinding tool, is put into discharge plasma sintering furnace,
Under 60MPa, 900 DEG C of insulation 5min are warming up to the speed of 60 DEG C/min, furnace cooling after the completion of sintering obtains block niobium silver and closes
Golden material.
Fig. 1 is the outside drawing of Nb80Ag20 alloy materials manufactured in the present embodiment, and the alloy material is a diameter of 10mm left
Right cylinder, its surfacing is bright and with metallic luster.
Fig. 2 is the scanning electron microscope (SEM) photograph of Nb80Ag20 alloy materials manufactured in the present embodiment, wherein white is Ag precipitated phases, secretly
Color is Nb matrixes.Silver-colored precipitated phase is evenly distributed, and crystallite dimension is a kind of Nanoalloy material between 20-200nm.
Embodiment 2
(1) in the glove box protected full of argon gas, by mole meter, by 0.5% silver powder and 99.5% niobium
Powder is mixed, and obtains mixed-powder, and the purity of niobium powder and silver powder is 99.99%；Mixed-powder is placed in high energy ball mill
In, it is 4 with the mass ratio of mixed-powder to control abrading-ball:1, high-energy ball milling 6h, obtain alloy powder；
(2) alloy powder that step (1) is obtained is placed in graphite grinding tool, is put into discharge plasma sintering furnace,
Under 100MPa, 800 DEG C of insulation 30min are warming up to the speed of 100 DEG C/min, furnace cooling after the completion of sintering obtains block niobium
Silver alloy.
Silver-colored precipitated phase is evenly distributed in niobium silver alloy manufactured in the present embodiment, crystallite dimension between 20-230nm,
It is a kind of Nanoalloy material.
Embodiment 3
(1) in the glove box protected full of argon gas, by mole meter, the niobium powder of 5% silver powder and 95% is entered
Row mixing, obtains mixed-powder, and the purity of niobium powder and silver powder is 99.99%；Mixed-powder is placed in high energy ball mill, is controlled
Abrading-ball processed is 10 with the mass ratio of mixed-powder:1, high-energy ball milling 20h, obtain alloy powder；
(2) alloy powder that step (1) is obtained is placed in graphite grinding tool, is put into discharge plasma sintering furnace,
Under 10MPa, 900 DEG C of insulation 1min are warming up to the speed of 50 DEG C/min, furnace cooling after the completion of sintering obtains block niobium silver and closes
Golden material.
Silver-colored precipitated phase is evenly distributed in niobium silver alloy manufactured in the present embodiment, crystallite dimension between 20-200nm,
It is a kind of Nanoalloy material.
Embodiment 4
(1) in the glove box protected full of helium, by mole meter, the niobium powder of 40% silver powder and 60% is entered
Row mixing, obtains mixed-powder, and the purity of niobium powder and silver powder is 99.99%；Mixed-powder is placed in high energy ball mill, is controlled
Abrading-ball processed is 6 with the mass ratio of mixed-powder:1, high-energy ball milling 1h, obtain alloy powder；
(2) alloy powder that step (1) is obtained is placed in graphite grinding tool, is put into discharge plasma sintering furnace,
Under 50MPa, 850 DEG C of insulation 20min are warming up to the speed of 80 DEG C/min, furnace cooling after the completion of sintering obtains block niobium silver
Alloy material.
Silver-colored precipitated phase is evenly distributed in niobium silver alloy manufactured in the present embodiment, crystallite dimension between 20-300nm,
It is a kind of Nanoalloy material.
Embodiment 5
(1) in the glove box full of argon gas and helium mix gas shield, by mole meter, by 20% silver powder
Niobium powder with 80% is mixed, and obtains mixed-powder, and the purity of niobium powder and silver powder is 99.99%；Mixed-powder is placed in
In high energy ball mill, it is 5 with the mass ratio of mixed-powder to control abrading-ball:1, high-energy ball milling 12h, obtain alloy powder；
(2) alloy powder that step (1) is obtained is placed in graphite grinding tool, is put into discharge plasma sintering furnace,
Under 60MPa, 900 DEG C of insulation 5min are warming up to the speed of 60 DEG C/min, furnace cooling after the completion of sintering obtains block niobium silver and closes
Golden material；
(3) the niobium silver alloy that step (2) is obtained is placed in vacuum drying oven, 600 is warming up to the speed of 10 DEG C/min
DEG C insulation 2h, natural cooling, obtain through annealing niobium silver alloy.
Fig. 3 is the scanning electron microscope (SEM) photograph of Nb80Ag20 alloy materials manufactured in the present embodiment, wherein white is Ag, dark-coloured matrix
It is Nb, compared with Fig. 2, crystallite dimension increase 20% or so after annealing.
Silver-colored precipitated phase is evenly distributed in niobium silver alloy manufactured in the present embodiment, crystallite dimension between 30-250nm,
It is a kind of Nanoalloy material.
Embodiment 6
(1) in the glove box protected full of argon gas, by mole meter, the niobium powder of 1% silver powder and 99% is entered
Row mixing, obtains mixed-powder, and the purity of niobium powder and silver powder is 99.99%；Mixed-powder is placed in high energy ball mill, is controlled
Abrading-ball processed is 7 with the mass ratio of mixed-powder:1, high-energy ball milling 3h, obtain alloy powder；
(2) alloy powder that step (1) is obtained is placed in graphite grinding tool, is put into discharge plasma sintering furnace,
Under 60MPa, 900 DEG C of insulation 5min are warming up to the speed of 60 DEG C/min, furnace cooling after the completion of sintering obtains block niobium silver and closes
Golden material；
(3) the niobium silver alloy that step (2) is obtained is placed in vacuum drying oven, 800 DEG C is warming up to the speed of 5 DEG C/min
Insulation 1h, natural cooling obtains the niobium silver alloy by making annealing treatment.
Silver-colored precipitated phase is evenly distributed in niobium silver alloy manufactured in the present embodiment, crystallite dimension between 30-300nm,
It is a kind of Nanoalloy material.
Embodiment 7
Compared with Example 1, " purity of niobium powder is except " purity of niobium powder and silver powder is 99.99% " is replaced with
99%, the purity of silver powder is 99% " outward, other conditions and all same of embodiment 1.
Silver-colored precipitated phase is evenly distributed in niobium silver alloy manufactured in the present embodiment, crystallite dimension between 20-250nm,
It is a kind of Nanoalloy material.
Comparative example 1
(1) in the glove box protected full of argon gas, by mole meter, the niobium powder of 10% silver powder and 90% is entered
Row mixing, obtains mixed-powder, and the purity of niobium powder and silver powder is 99.99%；Mixed-powder is placed in general milling machine, is controlled
Abrading-ball processed is 5 with the mass ratio of mixed-powder:1, ball milling 12h, obtain alloy powder；
(2) alloy powder that step (1) is obtained is placed in graphite grinding tool, is put into discharge plasma sintering furnace,
Under 60MPa, 900 DEG C of insulation 5min, furnace cooling after the completion of sintering are warming up to the speed of 100 DEG C/min.
High-energy ball milling is substituted with general milling.The uniform nanocrystalline niobium silver of microstructure can not be obtained after the completion of sintering to close
Golden material.
Comparative example 2
(1) with embodiment 1.
(2) alloy powder that step (1) is obtained is placed in conventional thermocompression sintering furnace, under 60MPa, with 10 DEG C/min's
Speed is warming up to 900 DEG C of insulation 1h, furnace cooling after the completion of sintering.
Replace discharge plasma with common hot pressed sintering to sinter, if with identical sintering condition, powder cannot be molded；
If the extension sintered heat insulating time, it is impossible to obtain nanocrystalline niobium silver alloy.
Comparative example 3
(1) in the glove box protected full of argon gas, by mole meter, the niobium powder of 10% silver powder and 90% is entered
Row mixing, obtains mixed-powder, and the purity of niobium powder and silver powder is 99.99%；
(2) mixed-powder that step (1) is obtained is placed in graphite grinding tool, is put into discharge plasma sintering furnace,
Under 60MPa, 900 DEG C of insulation 5min, furnace cooling after the completion of sintering are warming up to the speed of 60 DEG C/min.
High-energy ball milling is not carried out, and discharge plasma sintering is directly carried out after silver powder and niobium powder are mixed.Sintering is completed
After can not obtain the uniform niobium silver alloy of microstructure.
Performance test：
Performance test is carried out to niobium silver alloy prepared by embodiment of the present invention 1-7, test result is as shown in table 1.
(1) compressive strength of material is measured using omnipotent compression test；
(2) Vickers hardness is determined using Vickers hardness measuring instrument；
(3) electrochemical workstation is used, electrolyte is artificial saliva, and temperature is 25 DEG C of room temperature, and voltage range is open circuit electricity
Positive pressure bears 0.5mV, after obtaining polarization curve, according to Tafel equation, calculates corrosion potentials and corrosion current, obtains niobium silver and closes
The corrosion rate (being characterized with corrosion electric current density method) of gold；
(4) it is contrast with pure niobium material, according to the antibiotic rate of ASTM G21-96 standard testing niobium silver alloy.
Table 1
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned implementation method
Detail, in range of the technology design of the invention, various simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy is no longer separately illustrated.
Additionally, can also be combined between a variety of implementation methods of the invention, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of niobium silver alloy, it is characterised in that the niobium silver alloy presses molar content by following components group
Into：Niobium 60-99.95%, silver-colored 0.05-40%.
2. niobium silver alloy as claimed in claim 1, it is characterised in that the crystallite dimension of the niobium silver alloy is
20-300nm；
Preferably, the compressive strength of the niobium silver alloy is 1.0-1.8GPa；
Preferably, the Vickers hardness of the niobium silver alloy is 3.0-6.5GPa.
3. the preparation method of niobium silver alloy as claimed in claim 1 or 2, it is characterised in that methods described includes following
Step：
(1) under an inert atmosphere, silver powder and niobium powder are mixed to get mixed-powder, high energy ball is then carried out in high energy ball mill
Mill, obtains niobium silver solid solution alloy powder；
(2) alloy powder that step (1) is obtained is carried out into discharge plasma sintering, furnace cooling after the completion of sintering obtains block
Body niobium silver alloy.
4. method as claimed in claim 3, it is characterised in that the purity of step (1) the niobium powder is more than 99%, preferably
More than 99.99%；
Preferably, the purity of step (1) described silver powder is more than 99%, preferably more than 99.99%；
Preferably, abrading-ball and the mass ratio of mixed-powder are (4-10) in step (1) described Process During High Energy Ball Milling:1, preferably
(4-8):1, more preferably 5:1；
Preferably, the time of step (1) described high-energy ball milling is 1-50h.
5. the method as described in claim 3 or 4, it is characterised in that step (1) described inert gas is helium and/or argon gas；
Preferably, the rotational frequency of the fixture of step (1) described high energy ball mill is 15-20Hz, preferably 17Hz；
Preferably, the rotating speed of step (1) described high energy ball mill is 1600-1800r/min, preferably 1725r/min.
6. the method as described in claim any one of 3-5, it is characterised in that step (2) the discharge plasma sintering
Temperature is 800-950 DEG C；
Preferably, the time of step (2) the discharge plasma sintering is 1-30min；
Preferably, the pressure of step (2) the discharge plasma sintering is 10-100MPa；
Preferably, the heating rate of step (2) the discharge plasma sintering is 20-100 DEG C/min.
7. the method as described in claim any one of 3-6, it is characterised in that the block niobium silver alloy material obtained to step (2)
Material is made annealing treatment.
8. method as claimed in claim 7, it is characterised in that the annealing is in vacuum drying oven or the heat of inert gas shielding
Carried out in treatment furnace；
Preferably, the temperature of the annealing is 400-800 DEG C；
Preferably, the time of the annealing is 0.5-3h；
Preferably, the heating rate of the annealing is 5-50 DEG C/min；
Preferably, the inert gas is helium and/or argon gas.
9. the method as described in claim any one of 3-8, it is characterised in that the described method comprises the following steps：
(1) under an inert atmosphere, silver powder and niobium powder are mixed to get mixed-powder, then the high-energy ball milling 1- in high energy ball mill
50h, obtains niobium silver solid solution alloy powder；Wherein, the purity of the silver powder and niobium powder is more than 99%, the high-energy ball milling mistake
Abrading-ball and the mass ratio of mixed-powder are (4-10) in journey:1, the inert gas is helium and/or argon gas, the high-energy ball milling
The rotational frequency of machine clamp is 15-20Hz, and rotating speed is 1600-1800r/min；
(2) alloy powder that step (1) is obtained is carried out into discharge plasma sintering, block niobium silver alloy is obtained after the completion of sintering
Material；Wherein, the temperature of discharge plasma sintering is 800-950 DEG C, and the time of the discharge plasma sintering is
1-30min, the pressure of the discharge plasma sintering is 10-100MPa, the heating rate of the discharge plasma sintering
It is 20-100 DEG C/min；
(3) the block niobium silver alloy for obtaining step (2) is made annealing treatment；Wherein, the annealing is in vacuum drying oven
Or carried out in the heat-treatment furnace of inert gas shielding, the temperature of the annealing is 400-800 DEG C, the annealing when
Between be 0.5-3h, the heating rate of the annealing is 5-50 DEG C/min, and the inert gas is helium and/or argon gas.
10. niobium silver alloy as claimed in claim 1 or 2 as dental material application.
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