CN109464286A - A kind of dental Ti alloy and preparation method thereof - Google Patents
A kind of dental Ti alloy and preparation method thereof Download PDFInfo
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- CN109464286A CN109464286A CN201811441636.4A CN201811441636A CN109464286A CN 109464286 A CN109464286 A CN 109464286A CN 201811441636 A CN201811441636 A CN 201811441636A CN 109464286 A CN109464286 A CN 109464286A
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 98
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000010936 titanium Substances 0.000 claims abstract description 86
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 71
- 239000000956 alloy Substances 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 14
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 96
- 238000000034 method Methods 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 21
- 230000007704 transition Effects 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 4
- 239000010720 hydraulic oil Substances 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 238000005299 abrasion Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 26
- 239000000843 powder Substances 0.000 description 12
- 238000005266 casting Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910052573 porcelain Inorganic materials 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 210000000214 mouth Anatomy 0.000 description 3
- 238000003325 tomography Methods 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 230000035807 sensation Effects 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/70—Preparations for dentistry comprising inorganic additives
- A61K6/71—Fillers
-
- B22F1/0003—
-
- 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
- B22F3/02—Compacting only
-
- 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
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- 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
- B22F3/24—After-treatment of workpieces or articles
-
- 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
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- 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
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium 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
- 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
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
-
- 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
- B22F2207/00—Aspects of the compositions, gradients
- B22F2207/01—Composition gradients
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Mechanical Engineering (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Epidemiology (AREA)
- Physics & Mathematics (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Fluid Mechanics (AREA)
- Inorganic Chemistry (AREA)
- Materials For Medical Uses (AREA)
- Dental Preparations (AREA)
Abstract
The invention belongs to artificial tooth production fields, and in particular to a kind of dental Ti alloy and preparation method thereof.The specific technical proposal is: a kind of titanium alloy, including 35~45 parts of pure titaniums and 55~65 parts of titanium alloys;The mass fraction of each element in the pure titanium are as follows: Fe≤0.3%, C≤0.1%, N≤0.05%, H≤0.015%, O≤0.25%, remaining impurity≤0.4%, surplus Ti;The mass fraction of each element in the titanium alloy are as follows: 5.5%≤Al≤6.75%, 3.5≤V≤4.5%, Fe≤0.3%, C≤0.08%, N≤0.05%, H≤0.015%, O≤0.2%, remaining impurity≤0.4%, surplus Ti.The top of the alloy material is pure titanium material, and mechanical strength is low, for making the cut end and occlusal surface of artificial tooth, is contacted with to jaw, smaller to the abrasion of natural teeth.Middle part and bottom have larger intensity, and as the main structure of artificial tooth, satisfactory mechanical property can bear larger bite force;Good biocompatibility.
Description
Technical field
The invention belongs to artificial tooth production fields, and in particular to a kind of dental Ti alloy and preparation method thereof.
Background technique
Metal material currently used for oral artificial tooth reparation is mainly cochrome, pure titanium or titanium alloy.Cochrome because
It is lower for price, at the same the material for artificial tooth produce when, the common process of use --- casting technique, it is relatively simple and failure
Rate is lower, while cochrome can form good combination with existing porcelain powder, so having obtained largely in oral cavity industry
Using.But due to cochrome contains that the harmful elements such as nickel, density are high, casting technique is coarse etc. at it, lead to its biology
Compatibility is bad, and foreign body sensation is strong in mouth, and edge is closely sealed.
Pure titanium or titanium alloy material is due to good biocompatibility, and lower density, good processability is in tooth
The application range of section constantly expands.When pure titanium or titanium alloy material is used primarily for artificial tooth production, made using casting technique
Make to be preced with (outer layer does porcelain process) in the full anatomical crown of metal either metal.But the fusing point of titanium alloy is very high, simultaneously
The titanium chemistry of melting is very active, is easy to react with other substances and lose original physicochemical characteristics, by
More impurity are brought in chemical reaction, biocompatibility reduces.In addition, due to the inaccuracy of casting technique itself, titanium and
Its alloy is lower with the bond strength between existing porcelain powder, and porcelain operation is more complicated on this, collapses porcelain situation more in the later period mouthful
Seriously.The intensity of titanium alloy is high, and hardness is higher by much compared with natural teeth, generates biggish abrasion to the natural teeth to jaw.The above original
Because causing titanium and its alloy material to receive biggish inhibition in the application of dentistry.
The features such as dental Ti alloy is corrosion-resistant due to its good biocompatibility, and density is small, applied to medical industry
Advantage is that other many materials can not all replace, and there is no selections to abandon for market and industry.But we be badly in need of one kind can
Using high-precision processing technology, the titanium of human body needs is more in line with to change the status quo.CAD/CAM technology is introduced in dentistry
This change is had laid a good foundation.By means of machinery industry, the principle of numerically controlled machine tool.There is titanium in dentistry in market
Disk, dental Ti alloy disk.Titanium or titanium alloy material is made into the circular pan-like structure that can be clamped by numerically controlled machine tool, then will
It is imported into cutting software by the tooth three-dimensional data after CAD design, carries out typesetting, calculates, then cut.Due to
Mature accurate NC technology, truly can be converted to material object for virtual three-dimensional data.The method is solved due to casting
Original unmatched problem of tooth in technique bring low precision and mouth.But this dentistry titanium material, each specifications and models
All it is made of the titanium of the same trade mark.The titanium that the pure titanium and the trade mark that the mainly trade mark of the market mainstream is TA2 are TC4 closes
Gold.Different materials is selected according to different needs.Pure titanium is since purity is very high, and impurity content is very low, biocompatibility
Very well, while its hardness and strength is low, good toughness, is primarily adapted for use in movable support and complete solution cuts open metal crown.Titanium alloy is due to adding
Aluminium is added, the elements such as vanadium improve the mechanical strength of material, and the metal crown bridge class bigger suitable for stress, bar card, gantry class are repaired
Multiple type, but since its hardness increases simultaneously, the abrasion of natural teeth are increased simultaneously.
To sum up, industry is badly in need of a kind of good biocompatibility, and density is low, and foreign body sensation is weak, can bear biggish bite force, together
When to the abrasion of natural teeth low titanium material again.
Summary of the invention
The object of the present invention is to provide a kind of dental Ti alloys and preparation method thereof.
For achieving the above object, the technical scheme adopted by the invention is that: a kind of titanium alloy, with total weight be 100
Part meter, including 35~45 parts of pure titaniums and 55~65 parts of titanium alloys;The partial size of the pure titanium and titanium alloy is 100~120nm;
The mass fraction of each element in the pure titanium are as follows: Fe≤0.3%, C≤0.1%, N≤0.05%, H≤0.015%,
O≤0.25%, remaining impurity≤0.4%, surplus Ti;
The mass fraction of each element in the titanium alloy are as follows: 5.5%≤Al≤6.75%, 3.5≤V≤4.5%, Fe≤
0.3%, C≤0.08%, N≤0.05%, H≤0.015%, O≤0.2%, remaining impurity≤0.4%, surplus Ti.
Preferably, in the pure titanium, in addition to Ti, remaining element accounting total amount≤0.01%.
Preferably, in the titanium alloy, 5.5%≤Al≤6.5%, 3.5≤V≤4%, surplus Ti.
Correspondingly, a kind of method for preparing the titanium alloy, includes the following steps:
(1) gross mass weighs 20~24 parts of pure titanium and 33~34.2 parts of titanium alloys, as raw material based on 100 parts respectively
1,2;Transition zone raw material is used as after weighing remaining pure titanium and titanium alloy mixing;
(2) above-mentioned raw materials are sequentially placed into mold, by the sequence of raw material 2, transition zone raw material, raw material 1 at 50~60 tons
Pressure keeps 0.5h or more, and each raw material is tentatively pressed into the alloy material of required shape;
(3) alloy material is sealed again, is put into liquid, apply 200~230 tons of pressure to the liquid, kept
1h or more;
(4) alloy material is put into vacuum annealing furnace again, is warming up to 960~1200 DEG C with 10 DEG C/m speed,
Heat preservation 4~6 hours, is machined according to needed for after natural cooling.
Preferably, step (1) the transition zone raw material specific the preparation method comprises the following steps:
5~7 parts of pure titaniums and 5~7 parts of titanium alloys, and pure titanium and titanium alloy equivalent are weighed, raw material 3 is used as after mixing;Weigh 5
~7 parts of pure titaniums and 7.5~10.5 parts of titanium alloys, in mass ratio, pure titanium: titanium alloy=1:1.5 is used as raw material 4 after mixing;It weighs
5~7 parts of pure titaniums and 9.5~13.3 parts, in mass ratio, pure titanium: titanium alloy=1:1.9 is used as raw material 5 after mixing;
It is put into the sequence of mold successively are as follows: raw material 2, raw material 5, raw material 4, raw material 3, raw material 1.
Preferably, by mass fraction, it is two parts of 1:3, respectively raw material 31 and raw material 32 that the raw material 3, which is divided to,;It will be former
Expect three parts that 4 points are 1:1:2, respectively raw material 41, raw material 42 and raw material 43;It is two parts of 1:3 that raw material 5, which is divided to, respectively former
Material 51 and raw material 52;Raw material 31,41,42,51 is poured into mold respectively, keeps 5~10min using 10~20 tons of pressure, point
It is not pressed into the first connecting layer, the second connecting layer, third connecting layer and the 4th connecting layer, each connecting layer top and bottom are respectively at least
One connected structure is set;
It is put into the sequence of mold successively are as follows: raw material 2, the 4th connecting layer, raw material 5, third connecting layer, raw material 4, second are connected
Layer, raw material 3, the first connecting layer, raw material 1.
Preferably, each connecting layer is herring-bone form.
Preferably, the mixing method particularly includes: powder is poured into at least two volumes and is situated between in the liquid of powder total amount
In matter, after ultrasonic vibration >=10min, another side ultrasonic vibration is dry in≤65 DEG C of environment on one side, removes whole liquid and is situated between
To get required mixing raw material after matter;The liquid medium neither reacts with pure titanium or titanium alloy, does not also dissolve pure titanium and titanium
Alloy.
Preferably, the liquid medium is deionized water.
The invention has the following advantages:
Although 1, titanium or titanium alloy has many advantages, such as preferable biocompatibility, while also having that corrosion-resistant, density is small,
The problems such as pure titanium is lower there are hardness and strength, application places are limited.And the titanium that the elements such as aluminium, vanadium are increased in pure titanium closes
Gold, satisfactory mechanical property overcome the segmental defect of pure titanium, but simultaneously as its intensity is larger, there is also grind to natural teeth
The problems such as consumption increases.
Inventive formulation is simple, only uses common pure titanium and titanium alloy, in the case where being not added with other special materials, i.e.,
Dental titanium alloy both with a kind of hardness is provided, while meeting that artificial tooth is complicated and conflicting requirement;And this hair
Bright preparation process is also very simple easy to accomplish.The top of finally obtained alloy material is pure titanium material, and mechanical strength is low,
For making the cut end and occlusal surface of artificial tooth, contacted with to jaw, it is smaller to the abrasion of natural teeth.Middle part and bottom have larger strong
Degree, as the main structure of artificial tooth, satisfactory mechanical property can bear larger bite force;Good biocompatibility.
2, in the prior art, dental titanium alloy is improved, or metal alloy is improved, is all to provide one
It is more more uniform better to be intended to each element distribution for the alloy that kind each element is evenly distributed, but such alloy certainly will be only with single
Characteristic, multiple performance can not be had both simultaneously.The present invention overcomes the technology prejudice of this field, creatively provide a kind of each
The non-uniform alloy material of Elemental redistribution makes the alloy material have different characteristics in different location.
If the case where 3, simply being combined pure titanium and titanium alloy, just will appear junction tomography, junction is combined
It is not close, it is easy occur performance breakpoint in use.Pure titanium and titanium alloy are carried out well the present invention also provides a kind of
The method of transition bonding, is expanded to three-dimensional from two dimension for the intersection of pure titanium and titanium alloy, is expanded to solid from single side, effectively keeps away
The tomography problem of junction is exempted from.Meanwhile the pure titanium and titanium alloy of binding site form a kind of new transition material, it is not only simultaneous
Have the characteristic of pure titanium and titanium alloy, also there is certain buffering effect.
Detailed description of the invention
Fig. 1 is a kind of linking schematic diagram of a layer structure of the invention;
Fig. 2 is preferred linking schematic diagram of a layer structure of the invention;
Fig. 3 is alloy material interlayer structural schematic diagram of the present invention.
Specific embodiment
1, formula of the present invention: in an amount be 100 parts meter, inventive formulation include 35~45 parts pure titanium and 55~
65 parts of titanium alloy.The pure titanium and titanium alloy are powder, and partial size is 100~120nm.Partial size can not be then distributed greatly very much
It is even, and initial strength is lower after molding, bad mechanical property;The too small then mobility of partial size is excessively poor, is also difficult under pressure
Type.
Common commercially available raw material powder particle size is generally 40nm or so, and very uneven, and direct pressing is difficult to form,
And the uniformity is very low, is unable to satisfy requirement of the invention.Therefore, it if using commercially available pure titanium and titanium alloy, first will need
Powder and liquid gum are that 1:1 is mixed, then obtains coarse powder by spray drying process, then coarse powder is sieved in mass ratio, are obtained
To the raw material of required partial size.The liquid gum press mass fraction are as follows: 5% polyvinyl alcohol, 1% sodium carbonate (dispersion
Agent), surplus is water.Only it is to provide a kind of method of available required partial size herein, is not necessarily referring to the present invention and is limited to make
Use this method.
(1) pure titanium is preferably free of the pure titanium of any impurity element, but in view of in daily production and application pure titanium price it is higher,
It is not easy to obtain, so the pure titanium containing certain impurity also can be used.Mainstream for convenience of operation, such as currently on the market is pure
Titanium, trade mark TA2.Through detecting, the mass fraction of each element in the pure titanium are as follows: Fe≤0.3%, C≤0.1%, N≤0.05%, H
≤ 0.015%, O≤0.25%, other impurities element summation≤0.4% and single content≤0.1%, surplus Ti.In principle,
As long as pure titanium quality is not less than the quality of above-mentioned TA2, goal of the invention may be implemented.
(2) titanium alloy preferably contains only tri- kinds of elements of Al, Ti, V, and presses mass fraction, 5.5%≤Al≤6.5%,
3.5≤V≤4%, surplus Ti.If cost may be higher in view of only using such alloy, contain so also can be used
There is the titanium alloy of certain impurity.Such as mainstream titanium alloy currently on the market, trade mark TC4.Through detecting, each member in the titanium alloy
The mass fraction of element are as follows: 5.5%≤Al≤6.75%, 3.5%≤V≤4.5%, Fe≤0.3%, C≤0.08%, N≤
0.05%, H≤0.015%, O≤0.2%, remaining impurity element summation≤0.4% and single contaminant element≤0.1%, surplus
For Ti.Quality is better than or is equal to the titanium alloy of TC4, can reach goal of the invention of the invention.
2, of the invention the preparation method comprises the following steps:
(1) the pure titanium and 33~34.2 parts of titanium alloys for weighing 20~24 parts respectively, as raw material 1,2;Weigh 5~7 parts it is pure
Titanium and 5~7 parts of titanium alloys (pure titanium and titanium alloy equivalent), are used as raw material 3 after mixing;Weigh 5~7 parts of pure titaniums and 7.5~10.5
Part titanium alloy (in mass ratio, pure titanium: titanium alloy=1:1.5) is used as raw material 4 after mixing;Weigh 5~7 parts of pure titaniums and 9.5~
13.3 parts of titanium alloys (in mass ratio, pure titanium: titanium alloy=1:1.9) are used as raw material 5 after mixing.
The mixing method particularly includes: the pure titanium of required mixing, titanium alloy raw material powder are poured into at least two volumes
In the deionized water of powder total amount, or pour into it is other do not reacted with pure titanium or titanium alloy, do not dissolve yet pure titanium or titanium alloy and
It is easy in evaporation/distillation liquid medium, after ultrasonic vibration 10min, (≤65 DEG C) dryings of another side ultrasonic vibration one side low temperature,
To get required mixing raw material after the whole liquid mediums of removal.It certainly, can also be straight when using water as liquid medium
Freeze-drying removal is connect, such as uses commercially available metal powder freeze dryer etc..It is of course also possible to using common mixing method, such as directly
It connects and stirs and evenly mixs, only effect is not so good as the above method.
(2) being divided to the raw material 3 is two parts of 1:3, respectively raw material 31 and raw material 32;It is the three of 1:1:2 that raw material 4, which is divided,
Part, respectively raw material 41, raw material 42 and raw material 43;It is two parts of 1:3, respectively raw material 51 and raw material 52 that raw material 5, which is divided to,.Respectively
Raw material 31,41,42,51 is poured into mold, 5~10min is kept using 10~20 tons of pressure, as shown in Figure 1, being pressed into respectively
First connecting layer, the second connecting layer, third connecting layer and the 4th connecting layer.Each connecting layer top and bottom are respectively at least arranged one
Connected structure.As shown in Fig. 2, each connecting layer is preferably arranged to herring-bone form structure, so as in subsequent operation with remaining interlayer knot
It closes close.
(3) as shown in figure 3, above-mentioned raw materials are pressed raw material 2, the 4th connecting layer, raw material 5, third connecting layer, raw material 4, second
The sequence of connecting layer, raw material 3, the first connecting layer, raw material 1, is sequentially placed into mold, using 50~60 tons of pressure, keeps 0.5h
More than, each raw material is tentatively pressed into the alloy material of required shape.
Certainly, step (2), in (3), will can also directly weigh remaining pure titanium and titanium alloy after raw material 1,2 and mix and make
For the raw material of intermediate layer, then is directly poured into mold and suppressed by the sequence of raw material 2, transition zone raw material, raw material 3.But
The titanium alloy of this method preparation is easy to appear tomography, the titanium alloy effect stability prepared not as good as the above method.
(4) alloy material is sealed again, is put into liquid, apply 200~230 tons of pressure to the liquid, kept
1h or more makes it combine more uniform densification;The compactness extent according to needed for artificial tooth, total amount are that the raw material of 100g can be prepared
24~25cm3Alloy material.
Alloy material can be directly placed into polybag by the sealing vacuumizes sealing, and the liquid is biodegradable
Hydraulic oil, such as plant hydraulic oil or synthesis class hydraulic oil.
(5) alloy material is put into vacuum annealing furnace, under protection of argon gas, is warming up to 10 DEG C/min speed
960 DEG C, then 1200 DEG C are warming up to the speed of 5 DEG C/min, keep the temperature 4~6 hours.
(6) it anneals and completes to the alloy material, then be down to 200 DEG C hereinafter, then natural again with the speed of 10 DEG C/min
Cooling is to get required alloy material.The titanium alloy prepared in this way, internal structure is fine and close, and transitional region is not letter
The single layer structure that unijunction closes, but the three-dimensional transition region being made of the different new alloy material of lattice, in entire alloy material
Portion's transition is natural, is tightly combined, and has certain buffer capacity.Meanwhile the minimum density inside entire alloy material is promoted
To 4.5g/cm3。
(7) alloy material is machined again, reaches required size.In general, artificial tooth material
Material needs to be machined to the accurate dimension and shape that carving milling equipment can clamp, such as φ 98mm, the shape with 2mm step.
Explanation is further expalined to the present invention below with reference to specific embodiment.
Embodiment one: influence of the impurity to titanium alloy performance
1,20 groups of alloy materials are prepared using above-mentioned formula and method, wherein liquid medium is water in the method for mixing, is done
Drying method is low temperature drying, and the structure of each connecting layer is herring-bone form structure.In vacuum annealing furnace, holding temperature is 1100 DEG C, is protected
The warm time is 4.5h.
The specific pure titanium and titanium alloy that each group uses are specifically as shown in table 1, and numerical value is mass percent in table, are lower than
0.01% element, which is considered as, to be ignored.Pure titanium: the ratio of titanium alloy is mass ratio, such as 9:13, that is, is corresponded in 100 parts of total amount, pure
Titanium accounts for 45 parts, and titanium alloy accounts for 65 parts.
The other design parameter table of 1 each group of table
2, above-mentioned 20 groups of titanium alloys are prepared as 5 × 5cm3Cube, be tested for the property, the results are shown in Table 2.Its
In, wear-resisting property is embodied with hardness, is detected by GB/T231.1-2009.Applicant in practice, it has been found that upper surface conjunction
The hardness control of golden material can satisfy mechanical property requirements in 200~290HB, and minimum to natural odontotripsis.Because in the presence of
Individual difference, the hardness that everyone is suitable for is different, and in general, the upper surface of titanium alloy controls in above-mentioned hardness range
It is attained by preferable effect.The present embodiment also provides kinds of schemes, can provide different hardness, can give birth in specific works
The titanium alloy of different hardness is produced to adapt to different situations.
The hardness of alloy material lower surface is controlled in 293~360HB, and more leveling off to, 360HB effect is better (to level off to general
The highest hardness of logical TC4 titanium alloy);Hardness is bigger, and intensity is bigger, can be born in processing with smaller thickness bigger
Power, meanwhile, hardness is bigger, and toughness accordingly reduces, and when processing is also not easy to adhere to cutter, and difficulty of processing reduces and machining accuracy mentions
It is high.
The other performance of 2 each group of table is shown
Embodiment two: influence of the index technique to titanium alloy performance
1,17 groups of alloy materials are prepared using above-mentioned formula and method, formula selects the group 1 of embodiment one.The tool of each group
Preparation process, parameter, as shown in table 3;Wherein, it is pre-stamped refer to first make the re-compacted molding of each connecting layer, do not carry out precompressed
System refer to each raw material add in order after direct pressing molding.
The other technological parameter of 3 each group of table
2, above-mentioned 17 groups of titanium alloys are prepared as 5 × 5cm3Cube, be tested for the property, the results are shown in Table 4.
The other performance of 4 each group of table is shown
Claims (10)
1. a kind of titanium alloy, it is characterised in that: be in terms of 100 parts by total weight, including 35~45 parts of pure titaniums and 55~65 parts of titaniums close
Gold;The partial size of the pure titanium and titanium alloy is 100~120nm;
The mass fraction of each element in the pure titanium are as follows: Fe≤0.3%, C≤0.1%, N≤0.05%, H≤0.015%, O≤
0.25%, remaining impurity≤0.4%, surplus Ti;
The mass fraction of each element in the titanium alloy are as follows: 5.5%≤Al≤6.75%, 3.5≤V≤4.5%, Fe≤0.3%,
C≤0.08%, N≤0.05%, H≤0.015%, O≤0.2%, remaining impurity≤0.4%, surplus Ti.
2. titanium alloy according to claim 1, it is characterised in that: in the pure titanium, in addition to Ti, remaining element accounting is total
Amount≤0.01%.
3. titanium alloy according to claim 1 or 2, it is characterised in that: in the titanium alloy, 5.5%≤Al≤6.5%,
3.5≤V≤4%, surplus Ti.
4. a kind of method for preparing titanium alloy described in claim 1, characterized by the following steps:
(1) gross mass weighs 20~24 parts of pure titanium and 33~34.2 parts of titanium alloys, as raw material 1,2 based on 100 parts respectively;
Transition zone raw material is used as after weighing remaining pure titanium and titanium alloy mixing;
(2) above-mentioned raw materials are sequentially placed into mold, by the sequence of raw material 2, transition zone raw material, raw material 1 in 50~60 tons of pressure
0.5h or more is kept, each raw material is tentatively pressed into the alloy material of required shape;
(3) alloy material is sealed again, is put into liquid, 200~230 tons of pressure is applied to the liquid, keep 1h with
On;
(4) alloy material is put into vacuum annealing furnace again, is warming up to 960~1200 DEG C with 10 DEG C/m speed, heat preservation 4
It~6 hours, is machined according to needed for after natural cooling.
5. a kind of method for preparing titanium alloy described in claim 1 according to claim 4, it is characterised in that: step (3)
The liquid is The Research Work On Bio-degradable Hydraulic Oil.
6. a kind of method for preparing titanium alloy described in claim 1 according to claim 4, it is characterised in that: step (1)
The transition zone raw material specific the preparation method comprises the following steps:
5~7 parts of pure titaniums and 5~7 parts of titanium alloys, and pure titanium and titanium alloy equivalent are weighed, raw material 3 is used as after mixing;Weigh 5~7
The pure titanium of part and 7.5~10.5 parts of titanium alloys, in mass ratio, pure titanium: titanium alloy=1:1.5 is used as raw material 4 after mixing;Weigh 5~
7 parts of pure titaniums and 9.5~13.3 parts of titanium alloys, in mass ratio, pure titanium: titanium alloy=1:1.9 is used as raw material 5 after mixing;
It is put into the sequence of mold successively are as follows: raw material 2, raw material 5, raw material 4, raw material 3, raw material 1.
7. a kind of method for preparing titanium alloy described in claim 1 according to claim 6, it is characterised in that: press quality
Number, it is two parts of 1:3, respectively raw material 31 and raw material 32 that the raw material 3, which is divided to,;It is three parts of 1:1:2 that raw material 4, which is divided, point
It Wei not raw material 41, raw material 42 and raw material 43;It is two parts of 1:3, respectively raw material 51 and raw material 52 that raw material 5, which is divided to,;It respectively will be former
Material 31,41,42,51 pours into mold, keeps 5~10min using 10~20 tons of pressure, is pressed into the first connecting layer, the respectively
A connected structure is respectively at least arranged in two connecting layers, third connecting layer and the 4th connecting layer, each connecting layer top and bottom;
Be put into the sequence of mold successively are as follows: raw material 2, the 4th connecting layer, raw material 5, third connecting layer, raw material 4, the second connecting layer,
Raw material 3, the first connecting layer, raw material 1.
8. a kind of method for preparing titanium alloy described in claim 1 according to claim 7, it is characterised in that: described each
Connecting layer is herring-bone form.
9. a kind of method for preparing titanium alloy described in claim 1, feature according to claim 4~8 any one
It is: the mixing method particularly includes: the substance of required mixing is poured into at least two volumes in substance total amount to be mixed
In liquid medium, after ultrasonic vibration >=10min, another side ultrasonic vibration is dry in≤65 DEG C of environment on one side, and removal is all
To get required mixing raw material after liquid medium;The liquid medium neither reacts with pure titanium or titanium alloy, it is pure also not dissolve
Titanium or titanium alloy.
10. a kind of method for preparing titanium alloy described in claim 1 according to claim 9, it is characterised in that: the liquid
Body medium is deionized water.
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Denomination of invention: A layered dental titanium alloy material and its preparation method Effective date of registration: 20210604 Granted publication date: 20200424 Pledgee: Chengdu SME financing Company Limited by Guarantee Pledgor: CHENGDU BESMILE BIOTECHNOLOGY Co.,Ltd. Registration number: Y2021510000085 |