TiZrNbCuAg antibacterial alloy and preparation method thereof
阅读说明：本技术 一种TiZrNbCuAg抗菌合金及其制备方法 (TiZrNbCuAg antibacterial alloy and preparation method thereof ) 是由 张涛 鲍晓通 于 2021-06-02 设计创作，主要内容包括：本发明涉及一种TiZrNbCuAg抗菌合金及其制备方法。所述合金的分子式为Ti-(a)Zr-(b)Nb-(c)Cu-(d)Ag-(e),其中下标a,b,c,d,e表示各对应合金元素的原子百分数,30<a<80,0<b<40,0<c<40,0≤d≤20,0≤e≤20,且a+b+c+d+e＝100。所述制备方法包括：步骤一：配料；步骤二：真空电弧炉制备合金锭；步骤三：快速凝固制备合金。该合金具有高的强度、低的弹性模量、良好的耐腐蚀性能、良好的生物相容性和优异的抗菌性能,对于开发更适合植入的生物医用材料具有重要的理论和实际意义。(The invention relates to a TiZrNbCuAg antibacterial alloy and a preparation method thereof. The molecular formula of the alloy is Ti a Zr b Nb c Cu d Ag e Wherein the subscripts a, b, c, d, e represent the atomic percentages of the respective alloy elements, 30<a<80,0<b<40,0<c<D is more than or equal to 0 and less than or equal to 20, e is more than or equal to 0 and less than or equal to 20, and a + b + c + d + e is equal to 100. The preparation method comprises the following steps: the method comprises the following steps: preparing materials; step two: preparing an alloy ingot by a vacuum arc furnace; step three: rapid solidification for preparing alloy. The alloy has high strength, low elastic modulus, good corrosion resistance, good biocompatibility and excellent antibacterial property, and has important theoretical and practical significance for developing biomedical materials more suitable for implantation.)
1. The TiZrNbCuAg antibacterial alloy is characterized in that the molecular formula of the alloy is TiaZrbNbcCudAgeWherein the subscripts a, b, c, d, e represent the atomic percentages of the respective alloy elements, 30<a<80,0<b<40,0<c<D is more than or equal to 0 and less than or equal to 20, e is more than or equal to 0 and less than or equal to 20, and a + b + c + d + e is equal to 100.
2. According to claim 1The alloy is characterized in that the molecular formula of the alloy is Ti50Zr25Nb25、Ti50Zr25Nb20Cu5、Ti50Zr25Nb20Ag5Or Ti50Zr25Nb20Cu2.5Ag2.5。
3. The alloy of claim 1, wherein said alloy has a BCC single phase structure or a structure containing a majority of BCC phases.
4. The alloy according to claim 1, wherein the alloy has a yield strength of 1000 to 2000MPa, a fracture strength of 1200 to 2800MPa, an elastic modulus of 40 to 90GPa, a pitting potential of-600 to-50 mV, and an antibacterial rate of 50 to 99.9%.
5. Method for preparing an alloy according to any of claims 1 to 4, comprising the following steps:
the method comprises the following steps: ingredients
According to TiaZrbNbcCudAgeWeighing a titanium simple substance, a zirconium simple substance, a niobium simple substance, a copper simple substance and a silver simple substance according to the target alloy components, uniformly mixing to obtain a smelting raw material, wherein the mass percentage purity of each element simple substance is not lower than 99.0%;
step two: preparation of alloy ingot by vacuum arc furnace
Putting the smelting raw materials weighed in the step one into a copper mould of a vacuum arc furnace, and vacuumizing to less than or equal to 5 multiplied by 10-3Pa, filling argon of 0.5Pa, and adjusting the vacuum degree to 0.5 Pa; arc melting is carried out under the protection atmosphere of argon with the mass percent purity of 99.999 percent, and Ti is obtained after being taken outaZrbNbcCudAgeAn alloy ingot;
step three: rapid solidification for preparing alloy
Ti prepared in the second stepaZrbNbcCudAgePutting the alloy ingot into an induction furnace of a rapid solidification device, and vacuumizingThe void degree is less than or equal to 1 multiplied by 10-1Pa, filling argon of 0.5Pa, and adjusting the vacuum degree to 0.5 Pa; completely melting the alloy, inducing current 15-20A, heating for 3-6 s, spray casting into copper mold, solidifying, and cooling to obtain TiaZrbNbcCudAgeAn alloy rod.
6. The method of claim 5, wherein in the second step, the arc melting parameter setting is as follows: the current is 50-120A, the smelting temperature is 1000-2500 ℃, the smelting time of each spindle is 2-3 minutes, and the smelting times are 4-5.
7. The method of claim 5, wherein in the third step, the injection molding pressure is 0.01-0.05 MPa.
8. The method of claim 5, wherein in the third step, the cooling rate is 10-10%3K/s。
Technical Field
The invention relates to a TiZrNbCuAg antibacterial alloy and a preparation method thereof, belonging to the field of preparation of antibacterial alloys.
Background
The TiZrNb alloy has low modulus and high strength, and the elementary substances of Cu and Ag have high antibacterial performance. The novel TiZrNbCuAg antibacterial alloy has high strength, low elastic modulus, excellent corrosion resistance, good biocompatibility and excellent antibacterial performance due to the special structure and element composition, so the novel TiZrNbCuAg antibacterial alloy has wide potential application value in the fields of antibacterial and bacteriostatic, bioimplantation, medical equipment and the like.
Disclosure of Invention
The technical problem of the invention is solved: the TiZrNbCuAg antibacterial alloy has high strength, low elastic modulus, excellent corrosion resistance, good biocompatibility and excellent antibacterial performance due to the special structure and element composition, so the TiZrNbCuAg antibacterial alloy has wide potential application value in the fields of antibacterial and bacteriostatic, bioimplantation, medical equipment and the like.
The invention is realized by the following technical scheme:
the molecular formula of the TiZrNbCuAg antibacterial alloy is TiaZrbNbcCudAgeWherein the subscripts a, b, c, d, e represent the atomic percentages of the respective alloy elements, 30<a<80,0<b<40,0<c<D is more than or equal to 0 and less than or equal to 20, e is more than or equal to 0 and less than or equal to 20, and a + b + c + d + e is equal to 100.
Further, the molecular formula of the alloy is Ti50Zr25Nb25、Ti50Zr25Nb20Cu5、Ti50Zr25Nb20Ag5Or Ti50Zr25Nb20Cu2.5Ag2.5。
Further, the alloy has a BCC single-phase structure or a structure containing a majority of BCC phase.
Furthermore, the alloy has the yield strength of 1000-2000 MPa, the breaking strength of 1200-2800 MPa, the elastic modulus of 40-90GPa, the pitting potential of-600-50 mV and the antibacterial rate of 50-99.9%.
A method of making an alloy as described in any preceding claim, comprising the steps of:
the method comprises the following steps: ingredients
According to TiaZrbNbcCudAgeWeighing a titanium simple substance, a zirconium simple substance, a niobium simple substance, a copper simple substance and a silver simple substance according to the target alloy components, uniformly mixing to obtain a smelting raw material, wherein the mass percentage purity of each element simple substance is not lower than 99.0%;
step two: preparation of alloy ingot by vacuum arc furnace
Putting the smelting raw materials weighed in the step one into a copper mould of a vacuum arc furnace, and vacuumizing to less than or equal to 5 multiplied by 10-3Pa, filling argon of 0.5Pa, and adjusting the vacuum degree to 0.5 Pa; arc melting is carried out under the protection atmosphere of argon with the mass percent purity of 99.999 percent, and Ti is obtained after being taken outaZrbNbcCudAgeAn alloy ingot;
step three: rapid solidification for preparing alloy
Ti prepared in the second stepaZrbNbcCudAgePlacing the alloy ingot into an induction furnace of a rapid solidification device, and vacuumizing to less than or equal to 1 multiplied by 10-1Pa, filling argon of 0.5Pa, and adjusting the vacuum degree to 0.5 Pa; completely melting the alloy, inducing current 15-20A, heating for 3-6 s, spray casting into copper mold, solidifying, and cooling to obtain TiaZrbNbcCudAgeAn alloy rod.
Further, in the second step, setting arc melting parameters: the current is 50-120A, the smelting temperature is 1000-2500 ℃, the smelting time of each spindle is 2-3 minutes, and the smelting times are 4-5.
Furthermore, in the third step, the injection casting pressure is 0.01-0.05 MPa.
Further, in the third step, the cooling rate is 10-103K/s。
The invention also provides a method for preparing the antibacterial alloy bar. The method comprises the steps of firstly weighing required pure elements of each simple substance according to target components, smelting the pure elements in a vacuum arc smelting furnace uniformly to obtain a master alloy ingot, and then manufacturing the alloy rod by using rapid solidification equipment and adopting a casting process.
Ti of the inventionaZrbNbcCudAgeThe alloy has the advantages that: the content of Cu and Ag elements is 0-20 at.%, the yield strength is 1000-2000 MPa, the fracture strength is 1200-2800 MPa, the elastic modulus is 40-90GPa, the pitting potential is-600-50 mV, and the antibacterial rate is 50-99.9%.
Drawings
FIG. 1 shows Ti of the present invention50Zr25Nb20Cu2.5 Ag2.5、Ti50Zr25Nb20Ag5And Ti50Zr25Nb22Cu3XRD pattern of the alloy;
FIG. 2 shows Ti of the present invention50Zr25Nb22Cu3The compressive stress-strain curve of the alloy;
FIG. 3 shows Ti of the present invention50Zr25Nb22 Cu3Potentiodynamic polarization curve of the alloy;
FIG. 4 shows Ti of the present invention50Zr25Nb20Ag5The compressive stress-strain curve of the alloy;
FIG. 5 shows Ti of the present invention50Zr25Nb20Ag5Potentiodynamic polarization curve of the alloy;
FIG. 6 shows Ti of the present invention50Zr25Nb20Cu2.5Ag2.5The compressive stress-strain curve of the alloy;
FIG. 7 shows Ti of the present invention50Zr25Nb22Cu3Alloy, Ti50Zr25Nb20Ag5Alloy, Ti50Zr25Nb20Cu2.5Ag2.5The colony count of the alloy and Ti-6Al-4V alloy.
Detailed Description
The invention is described in detail below with reference to the figures and the embodiments. The following examples are only for explaining the present invention, the scope of the present invention shall include the full contents of the claims, and the full contents of the claims of the present invention can be fully realized by those skilled in the art through the following examples.
The test apparatus and test method used in the following examples 1-3 were as follows:
(A) x-ray diffraction (XRD) analysis: the X-ray diffractometer adopted is D/MAX-2200pc, the manufacturer is Japan science, and the used target material is Cu target (Kalpha ray wavelength)) The sample is fixed in the central area of the sample frame by using plasticine, the sample is lightly pressed by using a glass sheet, the surface of the sample and the sample frame are ensured to be positioned on the same horizontal plane, and the set parameters are as follows: the working voltage is 40KV, the working current is 40mA, the scanning speed is 6 °/min, and the scanning angle range is 20 ° -120 °.
(B) Compressive stress strain curve of the alloy: the quasi-static compression experiment is carried out on a material universal testing machine, the model is SANS 550450KN, a rod-shaped alloy sample with the diameter of 2mm is adopted, and the length-diameter ratio of the sample is about 2: 1, two ends of a sample are ground to be parallel to each other and vertical to the axis of the sample in the experimental process through displacement control, and the loading test speed is 2.1 multiplied by 10 < -4 > s < -1 >. And calculating the yield strength, the breaking strength and the elastic modulus through the obtained stress-strain curve.
(C) Alloy potentiodynamic polarization curve: electrochemical testing was done in electrochemical workstations, Model Princeton Applied Research Model Versa STAT and Versa STAT 3. A three-electrode system is adopted, wherein an alloy sample is taken as a Working Electrode (WE), a platinum sheet is taken as a Counter Electrode (CE), a Saturated Calomel Electrode (SCE) is taken as a reference electrode, and a solution is (phosphate buffer solution, NaCl-8.01, KCl-0.20 and Na2HPO4-1.15，KH2PO40.20, units g/L) PBS solution. A sample with the diameter of 5mm and the thickness of 2mm of the alloy is soaked in a solution until the Open Circuit Potential (OCP) reaches a stable state, and then polarization experiments are carried out, wherein the polarization experiments comprise potentiodynamic polarization or cyclic anodic polarization. Potentiodynamic polarization scanning was started at 50mV below the open circuit potential (OCP-50mV), the stop potential was set at 2.0V, and the experiment was manually stopped after pitting occurredThe potential scan rate was 50 mV/min.
(D) The antibacterial rate of the alloy is as follows: the concentration is 1.5X 106cells/ml staphylococcus aureus ATCC25923(S. aureus) bacterial liquid 1ml is added into a 24-well plate, and an alloy sample with the diameter of 2mm and the length of 6mm is placed into each hole of the 24-well plate and is completely immersed in the bacterial liquid. After the 24-well plate was placed in a 37 ℃ incubator and incubated for 24 hours, a sample was taken out. The bacterial solution in each culture well, which had been immersed in the sample, was treated with PBS (phosphate buffer, NaCl-8.01, KCl-0.20, Na)2HPO4-1.15，KH2PO40.20 in g/L) was diluted in a gradient of 1:100, 1:1000 and 1: 10000. And (3) sucking 100 mu l of diluted bacteria liquid, dropwise adding the diluted bacteria liquid to a nutrient agar plate, uniformly coating the plate, putting the plate into a constant-temperature incubator at 37 ℃, culturing for 24 hours, and growing macroscopic dispersed colonies on the surface of the agar plate, wherein each single colony represents a single bacterium in the original sample. And recording the colony numbers in the culture dishes acted by different samples by using a digital camera, and comparing the colony numbers with a negative control group to calculate the bacteriostasis rate. Ti-6Al-4V alloy was used as a control.
Example 1
Preparation of Ti50Zr25Nb22Cu3Alloy (I)
The method comprises the following steps: ingredients
According to Ti50Zr25Nb22Cu3Weighing 3.000g of niobium simple substance, 3.347g of zirconium simple substance, 3.514g of titanium simple substance and 0.280g of copper simple substance in nominal components of the solid solution alloy, uniformly mixing to obtain smelting raw materials to form Ti50Zr25Nb22Cu310.141g of raw material of alloy; the purity of each element simple substance weighed by mass percent is equal to 99.9 percent.
Step two: preparation of alloy ingot by vacuum arc furnace
Putting the smelting raw materials weighed in the step one into a copper mould of a vacuum arc furnace (Nixin technical research NEW-ADR-05 type), and vacuumizing to 5 x 10-3Pa, filling argon of 0.5Pa, and regulating the pressure to 0.5Pa in vacuum; arc melting is carried out under the argon protective atmosphere with the mass percent purity of 99.999 percent, and the arc melting parameters are set as follows: current 120A, melting temperatureThe degree is 2200 ℃, the melting time of each spindle is 2 minutes, and the melting times are 4 times. Taking out to obtain Ti50Zr25Nb22Cu3And (3) alloy ingots.
Step three: rapid solidification preparation alloy bar
Ti prepared in the second step50Zr25Nb24Cu3The alloy ingot was placed in a rapid solidification apparatus (Nisshin Tech Co., Ltd., model No. NEW-A05), and the degree of vacuum was increased to 1X 10-1Pa, filling argon of 0.5Pa, and regulating the pressure to 0.5Pa in vacuum; heating for 5s under a current of 15A to completely melt the Ti, and spray-casting into a copper mold to solidify and cool to obtain Ti with a diameter of 2mm50Zr25Nb22Cu3An alloy rod; wherein, the spray casting pressure is 0.01 MPa; cooling rate of 103K/s, cooling to room temperature.
Ti obtained in example 150Zr25Nb22Cu3The alloy rods were analyzed by X-ray diffraction (XRD) and analyzed (test apparatus and test method as described in the foregoing test apparatus and test method (a)) to have a BCC single-phase solid solution structure, and the results are shown in fig. 1. The quasi-static compression test was performed on a material universal tester, and the obtained compressive stress-strain curve (the test apparatus and the test method are as described in the test apparatus and the test method (B)) was shown in fig. 2; and calculating the yield strength, the breaking strength and the elastic modulus through the obtained stress-strain curve. The potentiodynamic polarization curve of the alloy was measured by the three-electrode method (the test apparatus and test method are as described in the foregoing test apparatus and test method (C)), and the results are shown in fig. 3. The antibacterial ratio of the alloy (the test apparatus and the test method are as described in the foregoing test apparatus and test method (D)) was tested by culturing staphylococcus aureus on the surface of the alloy, washing off the surface of the staphylococcus aureus after seven days and culturing in a petri dish for 48 hours, and the results of the number of colonies are shown in fig. 7.
In FIG. 1Ti50Zr25Nb22Cu3The XRD pattern of the alloy shows that the alloy is a BCC single-phase structure by comparing diffraction peak positions. In FIG. 2 Ti50Zr25Nb22Cu3Compressive stress-strain curve of the alloy, canSo that the alloy has the yield strength of 1500MPa, the breaking strength of 2260MPa, the elastic modulus of 60GPa and good plasticity. In FIG. 3 Ti50Zr25Nb22Cu3The alloy has no pitting corrosion and the self-corrosion potential is-185 mv. From the colony count obtained in fig. 7, the antibacterial ratio of the alloy was calculated to be 75.9%.
Other alloy compositions of the present invention, prepared in the same manner as in example 1, are shown in table 1 below:
TABLE 1
Element(s)
Ti
Zr
Nb
Cu
Component A
40
10
49
1
Component two
40
20
37
3
Ingredient III
40
30
25
5
Ingredient four
40
40
13
7
Ingredient five
50
20
20
10
Ingredient six
50
15
20
15
Ingredient seven
50
15
15
20
Ingredient eight
60
15
15
10
Ingredient nine
70
10
15
5
Ingredient ten
80
7
10
3
Example 2
Preparation of Ti50Zr25Nb20Ag5Alloy (I)
The method comprises the following steps: ingredients
According to Ti50Zr25Nb20Ag5Weighing 3.000g of niobium simple substance, 3.682g of zirconium simple substance, 3.865g of titanium simple substance and 0.871g of silver simple substance in nominal components of solid solution alloy, uniformly mixing to obtain smelting raw materials to form Ti50Zr25Nb20Ag511.418g of raw material of alloy; the purity of each element simple substance weighed by mass percent is equal to 99.9 percent.
Step two: preparation of alloy ingot by vacuum arc furnace
Putting the smelting raw materials weighed in the step one into a copper mould of a vacuum arc furnace (Nixin technical research NEW-ADR-05 type), and vacuumizing to 5 x 10-3Pa, filling argon of 0.5Pa, and regulating the pressure to 0.5Pa in vacuum; arc melting is carried out under the argon protective atmosphere with the mass percent purity of 99.999 percent, and the arc melting parameters are set as follows: the current is 120A, the melting temperature is 1700 ℃, the melting time of each spindle is 2 minutes, and the melting times are 4. Taking out to obtain Ti50Zr25Nb20Ag5And (3) alloy ingots.
Step three: rapid solidification preparation alloy bar
Ti prepared in the second step50Zr25Nb20Ag5The alloy ingot was placed in a rapid solidification apparatus (Nisshin Tech Co., Ltd., model No. NEW-A05), and the degree of vacuum was increased to 1X 10-1Pa, filling argon of 0.5Pa, and vacuum-adjusting to 0.5 Pa; heating for 5s with a complete melting current of 15A, and solidifying in a copper mold by spray castingCooling to obtain Ti with the diameter of 2mm50Zr25Nb20Ag5An alloy rod; wherein, the spray casting pressure is 0.01 MPa; cooling rate of 103K/s, cooling to room temperature.
Ti obtained in example 250Zr25Nb20Ag5The alloy rods were analyzed by X-ray diffraction (XRD) and the test instruments and test methods were as described in the foregoing test instruments and test method (a) into BCC single-phase solid solution structures, and the results are shown in fig. 1. The quasi-static compression test was performed in a material universal tester, and the results of the obtained compressive stress-strain curve (the test apparatus and the test method are as described in the test apparatus and the test method (B)) are shown in fig. 2; the yield strength, breaking strength and elastic modulus were calculated from the obtained stress-strain curve, and the results are shown in fig. 4. The potentiodynamic polarization curve of the alloy was measured by the three-electrode method (the test apparatus and test method are as described in the foregoing test apparatus and test method (C)), and the results are shown in fig. 5. The antibacterial ratio of the alloy (the test apparatus and the test method are as described in the foregoing test apparatus and test method (D)) was tested by culturing staphylococcus aureus on the surface of the alloy, washing off the surface staphylococcus aureus after seven days and culturing in a petri dish for 48 hours, and the results are shown in fig. 7.
FIG. 1 is Ti50Zr25Nb20Ag5Comparing the diffraction peak positions by an XRD pattern, the alloy is a BCC single-phase structure. FIG. 4 is Ti50Zr25Nb20Ag5The compressive stress-strain curve of the alloy shows that the yield strength of the alloy is 1500MPa, the breaking strength is 2260MPa, the elastic modulus is 60GPa, and the alloy has good plasticity. FIG. 5 is Ti50Zr25Nb20Ag5The zeta potential polarization curve of the alloy has a self-corrosion potential of-245 mv, and no pitting corrosion phenomenon is found. From the colony count obtained in fig. 7, the antibacterial ratio of the alloy was calculated to be 84.6%.
Other alloy compositions of the present invention, prepared in the same manner as in example 1, are shown in Table 2 below:
TABLE 2
Example 3
Preparation of Ti50Zr25Nb20Cu2.5Ag2.5Alloy (I)
The method comprises the following steps: ingredients
According to Ti50Zr25Nb20Cu2.5Ag2.52.000g of niobium simple substance, 2.455g of zirconium simple substance, 2.577g of titanium simple substance, 0.171g of copper simple substance and 0.290g of silver simple substance are weighed according to nominal components of the alloy and are uniformly mixed to obtain smelting raw materials to form Ti50Zr25Nb20Cu2.5Ag2.57.493g of raw material of alloy; the mass percent purity of each selected element simple substance is equal to 99.9 percent.
Step two: preparation of alloy ingot by vacuum arc furnace
Putting the smelting raw materials weighed in the step one into a copper mould of a vacuum arc furnace (Nixin technical research NEW-ADR-05 type), and vacuumizing to 5 x 10-3Pa, filling argon of 0.5Pa, and regulating the pressure to 0.5Pa in vacuum; arc melting is carried out under the argon protective atmosphere with the mass percent purity of 99.999 percent, and the arc melting parameters are set as follows: the current is 80A, the melting temperature is 1200 ℃, the melting time of each spindle is 2 minutes, and the melting times are 4. Taking out to obtain Ti50Zr25Nb20Cu2.5Ag2.5And (3) alloy ingots.
Step three: fast solidification for preparing solid solution alloy
Ti prepared in the second step50Zr25Nb20Cu2.5Ag2.5The alloy ingot was placed in a rapid solidification apparatus (Nisshin Tech Co., Ltd., model No. NEW-A05), and the degree of vacuum was increased to 1X 10-1Pa, filling argon of 0.5Pa, and regulating the pressure to 0.5Pa in vacuum; melting completely with current 13A, heating for 4s, spray casting into copper mold, solidifying and cooling to obtain diameter2mm of Ti50Zr25Nb20Cu2.5Ag2.5An alloy rod; wherein the spray casting pressure is 0.01 MPa; cooling rate of 103K/s。
Ti obtained in example 350Zr25Nb20Cu2.5Ag2.5The alloy rods were analyzed by X-ray diffraction (XRD) and the test instruments and test methods were as described in the foregoing test instruments and test method (a) into BCC single-phase solid solution structures, and the results are shown in fig. 1. The quasi-static compression test was performed in a material universal tester, and the results of the obtained compressive stress-strain curve (the test apparatus and the test method are as described in the test apparatus and the test method (B)) are shown in fig. 6; and calculating the yield strength, the breaking strength and the elastic modulus through the obtained stress-strain curve.
FIG. 1Ti50Zr25Nb20Cu2.5Ag2.5Comparing the diffraction peak positions to obtain the alloy with BCC single-phase structure. FIG. 6 is Ti50Zr25Nb20Cu2.5Ag2.5As a compressive stress-strain curve of the alloy, the alloy has the advantages of 1500MPa of yield strength, 2260MPa of breaking strength, 60GPa of elastic modulus and good plasticity.
The antibacterial ratio of the alloy was tested by culturing staphylococcus aureus on the surface of the alloy, washing off the surface of the staphylococcus aureus after seven days and culturing in a petri dish for 48 hours (the test apparatus and the test method are as described in the test apparatus and the test method (D)) and the result is shown in fig. 7, which indicates that the alloy has excellent antibacterial performance.
Other alloy compositions of the present invention, prepared in the same manner as in example 3, are shown in Table 3 below:
TABLE 3
Element(s)
Ti
Zr
Nb
Cu
Ag
Component A
40
30
29
0
1
Component two
50
25
22
0
3
Ingredient III
60
20
15
0
5
Ingredient four
70
10
13
0
7
Ingredient five
50
25
20
4
1
Ingredient six
50
25
20
2.5
2.5
Ingredient seven
60
15
15
0
10
Ingredient eight
70
10
15
0
5
Ingredient nine
50
15
15
0
20
Ingredient ten
60
15
15
0
10
Ingredient eleven
70
10
15
0
5
Ingredient twelve
80
7
10
0
3
It should be noted that, according to the above embodiments of the present invention, those skilled in the art can fully implement the full scope of the present invention as defined by the independent claims and the dependent claims, and implement the processes and methods as the above embodiments; and the invention has not been described in detail so as not to obscure the present invention.
The above description is only a part of the embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
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