HK1071325B - Silver powder for silver clay and silver clay comprising the silver powder - Google Patents
Silver powder for silver clay and silver clay comprising the silver powder Download PDFInfo
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- HK1071325B HK1071325B HK05104296.8A HK05104296A HK1071325B HK 1071325 B HK1071325 B HK 1071325B HK 05104296 A HK05104296 A HK 05104296A HK 1071325 B HK1071325 B HK 1071325B
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Description
Technical Field
The present invention relates to a silver powder for silver clay having excellent low-temperature sinterability and a silver clay containing the silver powder.
Background
Silver ornaments or crafts are generally manufactured by casting or forging. In recent years, however, earth containing silver powder (Ag powder) has appeared on the market, and a method of manufacturing a silver ornament or a handicraft article having a predetermined shape by molding and sintering the silver clay into a predetermined shape has been proposed. According to the method, free-form molding can be performed using silver clay according to the same process as that of ordinary clay. Then, the molded article obtained by molding is dried and then sintered in a sintering furnace, and a silver ornament or a handicraft article can be very easily produced.
It is known that a conventional clay contains 50 to 95 mass% of a high-purity silver powder having an average particle diameter of 3 to 20 μm and a purity of 99.99 mass% or more, 0.8 to 8 mass% of a cellulose-based water-soluble binder, 0.1 to 3 mass% of an oil or fat, 0.03 to 3 mass% of a surfactant, and the balance being water (see Japanese patent application laid-open No. 4-26707).
When a molded article made of silver clay is dried and then sintered in an electric furnace, in the case of the silver clay of the prior art, a sintered body having sufficient strength cannot be obtained if the temperature is not maintained at or above the melting point of silver during sintering. The electric furnace used in the silver clay sintering can obtain a sintered body having a sufficient strength if it has the ability to maintain the temperature in the furnace at a relatively high temperature. However, many of the electric furnaces owned by individuals are small electric furnaces, have low heating capacity, and cannot maintain the furnace temperature at or above the melting point of silver, and therefore, there are cases where a sintered body having a sufficient density cannot be obtained.
Even in an electric furnace capable of maintaining a relatively high temperature, it is common that the temperature in the furnace cannot be accurately adjusted, and as a result, the temperature in the furnace becomes too high, and the sintered body is deformed.
Disclosure of Invention
Therefore, the present inventors have made studies in view of the above-mentioned problem that silver clay which can be sintered at a relatively low temperature can be obtained, and thus, sufficient sintering can be achieved even in a household electric furnace having a low heating capacity, and the control of the temperature in the electric furnace is relatively easy and easy at a low temperature, and that silver clay can be sintered at a low temperature without performing appropriate temperature control.
Based on this, the present inventors produced silver powder for silver clay containing 15 to 50 mass% of fine silver powder having an average particle diameter of 2 μm or less (preferably fine silver powder having an average particle diameter of 0.5 to 1.5 μm) and mixed with 50 to 85 mass% of silver powder having an average particle diameter of more than 2 μm and 100 μm or less (preferably silver powder having an average particle diameter of 3 to 20 μm), and then added an organic binder and other substances to the silver powder for silver clay to produce silver clay which can be sintered sufficiently at a temperature 250 to 410 ℃ lower than the melting point of pure silver (i.e., 550 to 710 ℃ lower) to obtain desired tensile strength and density.
The present invention has been accomplished based on this finding, and the present invention provides
(1) Silver powder for silver clay comprising a mixed powder containing 15 to 50 mass% of fine silver powder having an average particle diameter of 2 μm or less and the balance of silver powder having an average particle diameter of more than 2 μm and 100 μm or less, and
(2) a silver powder for silver clay comprising a mixed silver powder containing 15 to 50 mass% of a fine silver powder having an average particle diameter of 0.5 to 1.5 μm and the balance of silver powder having an average particle diameter of 3 to 20 μm.
Alternatively, the silver clay of the present invention is prepared by adding an organic binder or an organic binder, an oil or fat, a surfactant, etc. to the silver powder for silver clay (1) and (2). That is, the invention provides
(3) A silver clay containing 50 to 95 mass% of the silver powder for silver clay (1) or (2), 0.8 to 8 mass% of an organic binder, and the balance being water;
(4) a silver clay containing 50 to 95 mass% of the silver powder for silver clay (1) or (2), 0.8 to 8 mass% of an organic binder, 0.03 to 3 mass% of a surfactant, and the balance being water;
(5) a silver clay containing 50 to 95 mass% of the silver powder for silver clay (1) or (2), 0.8 to 8 mass% of an organic binder, 0.1 to 3 mass% of an oil, and the balance being water;
(6) a silver clay comprising 50 to 95 mass% of the silver powder for silver clay (1) or (2), 0.8 to 8 mass% of an organic binder, 0.1 to 3 mass% of an oil, 0.03 to 3 mass% of a surfactant, and the balance of water.
The fine silver powder having an average particle diameter of 2 μm or less contained in the silver powder for silver clay of the present invention is produced by a chemical reduction method or the like, and spherical fine silver powder is preferable. The reason why the content of the fine silver powder is limited to 15 to 50 mass% is that when the content of the fine silver powder having an average particle diameter of 2 μm or less is less than 15 mass%, the physical strength of the obtained sintered body is poor and is not satisfactory, and when the content of the fine silver powder having an average particle diameter of 2 μm or less exceeds 50 mass%, the amount of the organic binder is increased to achieve a clay state, and the shrinkage rate during sintering is increased, which is not satisfactory. When the average particle diameter is 2 μm or less, the content of the fine silver powder is more preferably 20 to 45% by mass.
Further, the remaining silver powder contained in the silver powder for silver clay of the present invention is a silver powder having an average particle diameter of more than 2 μm and not more than 100 μm, and if the average particle diameter is 2 μm or less, the physical strength of the sintered body is deteriorated, and if it exceeds 100 μm, the moldability of the clay is lowered.
In order to more easily understand the particle size distribution of the silver powder for silver clay of the present invention, the particle size distribution curve of the silver powder for silver clay shown in FIG. 1 is used for illustration. The silver powder for silver clay of the present invention is composed of a mixed silver powder formed by mixing a fine silver powder having an average particle diameter of 2 μm or less (preferably 0.5 to 1.5 μm, more preferably an average particle diameter of 0.6 to 1.2 μm) with a silver powder having an average particle diameter of 2 μm or more and 100 μm or less (preferably 3 to 20 μm, more preferably an average particle diameter of 3 to 8 μm). Therefore, the silver powder for silver clay of the present invention has a particle size distribution curve as shown by the solid line in FIG. 1, in which the fine silver powder having an average particle size of 2 μm or less (preferably 0.5 to 1.5 μm, more preferably 0.6 to 1.2 μm) has at least one peak A, and the silver powder having an average particle size of more than 2 μm and 100 μm or less (preferably 3 to 20 μm, more preferably 3 to 8 μm) has at least one peak B. That is, the silver powder for silver clay of the present invention has a particle size with at least two peaks A, B on the particle size distribution curve 1. On the other hand, since the silver powder for silver clay of the prior art has an average particle diameter of 3 to 20 μm, the particle size distribution thereof is shown by a dotted line in FIG. 1, and only one peak X is present on the particle size distribution curve 2. Therefore, the silver powder for silver clay of the present invention has a different particle size distribution compared to the silver powder for silver clay of the prior art.
Further, the average particle diameters of the fine silver powder and the silver powder constituting the silver powder for silver clay of the present invention are the average particle diameters of the fine silver powder and the silver powder not containing agglomerated powder agglomerates.
The reason why the content of the silver powder for silver clay (1) or (2) contained in the silver clay of the present invention is limited to 50 to 95% by mass is that when the content of the silver powder for silver clay is less than 50% by mass, the obtained sintered body cannot exhibit a sufficient metallic luster effect, and when it exceeds 95% by mass, the elongation and strength of the clay become undesirably low. The silver powder for silver clay is more preferably contained in an amount of 70 to 95 mass%.
The organic binder contained in the silver clay of the present invention may be a cellulose-based binder, a polyethylene-based binder, an acrylic-based binder, a wax-based binder, a resin-based binder, starch, gelatin, flour, or the like, and a cellulose-based binder, particularly water-soluble cellulose, is most preferable. These binders are added for the purpose of keeping the shape of the shaped article by rapidly gelling upon heating. If the amount of the organic binder added is less than 0.8% by mass, no effect is produced, and if it exceeds 8% by mass, fine cracks are formed in the obtained molded article, and the gloss is also lowered, which is not preferable. Therefore, the content of the binder in the silver clay of the present invention is 0.8 to 8% by mass. The content of the binder is more preferably 0.8 to 5% by mass.
The surfactant may be added as needed, and the amount of the surfactant added is preferably 0.03 to 3% by mass. The kind of the surfactant to be added is not particularly limited, and a general surfactant can be used.
The above-mentioned oil or fat may be added as needed, and the amount of the oil or fat added is preferably 0.1 to 3% by mass. The oil or fat to be added may be an organic acid (oleic acid, stearic acid, phthalic acid, palmitic acid, sebacic acid, acetyl citric acid, hydroxybenzoic acid, lauric acid, myristic acid, caproic acid, heptanoic acid, butyric acid, decanoic acid), an organic ester (an organic acid ester having methyl, ethyl, propyl, butyl, octyl, hexyl, dimethyl, diethyl, isopropyl, isobutyl), a higher alcohol (octanol, nonanol, decanol), a polyhydric alcohol (glycerol, arabitol, sorbitan), an ether (dioctyl ether, didecyl ether), or the like.
Brief Description of Drawings
FIG. 1 is a graph showing a particle size distribution of silver clay powder, which illustrates the difference between the silver powder for silver clay according to the present invention and the silver powder for silver clay according to the prior art.
FIG. 2 is a graph showing the relationship between the content of fine silver powder having an average particle diameter of 2 μm or less contained in clay and the density of a sintered body.
Detailed Description
Example 1
The ratio of the spherical silver fine powder having an average particle diameter of 1.0 μm produced by the chemical reduction method to the ultrafine silver powder having an average particle diameter of 5.0 μm was 0 mass%, 10 mass%, 20 mass%, 30 mass%, 40 mass%, 50 mass%, 60 mass%, 80 mass%, and 100 mass%, and these powders were mixed to produce 9 kinds of silver powder for silver clay having different particle sizes. Then, with respect to the silver powder for silver clay having the different particle size distribution of 9 kinds, methyl cellulose, a surfactant, olive oil as an oil and water were added to prepare silver clays 1 to 9 containing 85 mass% of the silver powder for silver clay, 4.5 mass% of methyl cellulose, 1.0 mass% of the surfactant, 0.3 mass% of olive oil, and the balance water.
These silver clays 1 to 9 were shaped, and the obtained shaped article was sintered at 600 ℃ for 30 minutes to produce test pieces having a thickness of 3mm, a width of 4mm and a length of 65mm, and the tensile strength and density of the sintered test pieces obtained were measured, and the measurement results are shown in table 1. Further, a curve is drawn by plotting Δ symbols on the vertical axis of the density measurement values in table 1 and the horizontal axis of the content of the spherical silver fine powder contained in the silver clay silver powder, and connecting these Δ symbols with a line, as shown in fig. 2.
TABLE 1
| Species of | Silver powder for silver clay | Sintered body of test piece | |||
| Average particle size: 1 micron spherical silver micro powder | Average particle size: 5 mu m superfine silver powder | Tensile Strength (N/mm)2) | Density (g/cm)3) | ||
| Silver clay | 1 | *- | 100 | 43 | 7.8 |
| 2 | *10 | Balance of | 45 | 7.9 | |
| 3 | 20 | Balance of | 80 | 8.5 | |
| 4 | 30 | Balance of | 100 | 8.7 | |
| 5 | 40 | Balance of | 75 | 8.6 | |
| 6 | 50 | Balance of | 73 | 8.2 | |
| 7 | *60 | Balance of | 51 | 7.8 | |
| 8 | *80 | Balance of | 42 | 7.2 | |
| 9 | *100 | - | 38 | 6.5 | |
(values outside the scope of the invention are indicated by symbols)
Example 2
The same procedure as in example 1 was repeated except that the ratio of the spherical fine silver powder having an average particle diameter of 1.5 μm produced by the chemical reduction method to the ultrafine silver powder having an average particle diameter of 5.0 μm was changed to 0 mass%, 10 mass%, 20 mass%, 30 mass%, 40 mass%, 50 mass%, 60 mass%, 80 mass%, and 100 mass%, and these powders were mixed to produce 9 kinds of silver powders for silver clay having different particle sizes, and the silver clays 10 to 18 were produced from the silver powders for silver clay having different particle size distributions of 9 kinds of particle sizes.
These silver clays 10 to 18 were shaped, the obtained shaped articles were sintered under the same conditions as in example 1 to produce test piece sintered bodies, and the tensile strength and density of the obtained test piece sintered bodies were measured in the same manner as in example 1, and the measured values are shown in table 2. Further, a graph is drawn by plotting points with symbols x on the vertical axis of the density measurement values in table 2 and the horizontal axis of the content of the spherical silver fine powder contained in the silver clay silver powder, and connecting these symbols x by lines, as shown in fig. 2.
TABLE 2
| Species of | Silver powder for silver clay | Sintered body of test piece | |||
| Average particle size: 1.5 μm spherical silver micro powder | Average particle size: 5 mu m superfine silver powder | Tensile Strength (N/mm)2) | Density (g/cm)3) | ||
| Silver clay | 10 | *- | 100 | 38 | 7.8 |
| 11 | *10 | Balance of | 51 | 7.7 | |
| 12 | 20 | Balance of | 90 | 8.4 | |
| 13 | 30 | Balance of | 95 | 8.5 | |
| 14 | 40 | Balance of | 73 | 8.3 | |
| 15 | 50 | Balance of | 70 | 8.1 | |
| 16 | *60 | Balance of | 50 | 7.7 | |
| 17 | *80 | Balance of | 43 | 7.3 | |
| 18 | *100 | - | 40 | 6.7 | |
(values outside the scope of the invention are indicated by symbols)
Example 3
The silver powders for 9 types of silver clay having different particle sizes were prepared by mixing 0 mass%, 10 mass%, 20 mass%, 30 mass%, 40 mass%, 50 mass%, 60 mass%, 80 mass% and 100 mass% of spherical fine silver powder having an average particle size of 0.5 μm produced by a chemical precipitation method with respect to ultrafine silver powder having an average particle size of 5.0 μm, and the silver clays 19 to 27 were prepared in the same manner as in example 1 using the silver powders for silver clay having different particle size distributions of 9 types.
These silver clays 19 to 27 were shaped, the obtained shaped articles were sintered under the same conditions as in example 1 to produce test piece sintered bodies, and the tensile strength and density of the obtained test piece sintered bodies were measured in the same manner as in example 1, and the measured values are shown in table 3. Further, a graph is drawn by plotting □ symbols on the vertical axis representing the density measurement values in table 3 and the horizontal axis representing the content of the spherical fine silver powder contained in the silver clay silver powder, and connecting these □ symbols with a line, as shown in fig. 2.
TABLE 3
| Species of | Silver powder for silver clay | Sintered body of test piece | |||
| Average particle size: 0.5 micron spherical silver micro powder | Average particle size: 5 mu m superfine silver powder | Tensile Strength (N/mm)2) | Density (g/cm)3) | ||
| Silver clay | 19 | *- | 100 | 39 | 7.7 |
| 20 | *10 | Balance of | 48 | 7.8 | |
| 21 | 20 | Balance of | 92 | 8.3 | |
| 22 | 30 | Balance of | 90 | 8.2 | |
| 23 | 40 | Balance of | 75 | 8.1 | |
| 24 | 50 | Balance of | 71 | 8.0 | |
| 25 | *60 | Balance of | 51 | 7.4 | |
| 26 | *80 | Balance of | 45 | 7.0 | |
| 27 | *100 | - | 35 | 6.5 | |
(values outside the scope of the invention are indicated by symbols)
Example 4
The silver powders for 9 types of silver clay having different particle sizes were prepared by mixing 0 mass%, 10 mass%, 20 mass%, 30 mass%, 40 mass%, 50 mass%, 60 mass%, 80 mass% and 100 mass% of spherical fine silver powder having an average particle size of 0.8 μm produced by a chemical precipitation method with respect to ultrafine silver powder having an average particle size of 5.0 μm, and silver clays 28 to 36 were prepared in the same manner as in example 1 using the silver powders for silver clay having different particle size distributions of 9 types.
These silver clays 28 to 36 were shaped, the obtained shaped articles were sintered under the same conditions as in example 1 to produce test piece sintered bodies, and the tensile strength and density of the obtained test piece sintered bodies were measured in the same manner as in example 1, and the measured values are shown in table 4. Further, a graph is drawn by plotting ● symbols on the vertical axis representing the density measurement values in table 4 and the horizontal axis representing the content of the spherical silver fine powder contained in the silver clay silver powder, and connecting these ● symbols with a line, as shown in fig. 2.
TABLE 4
| Species of | Silver powder for silver clay | Sintered body of test piece | |||
| Average particle size: 0.8 micron spherical silver micro powder | Average particle size: 5 mu m superfine silver powder | Tensile Strength (N/mm)2) | Density (g/cm)3) | ||
| Silver clay | 28 | *- | 100 | 40 | 7.7 |
| 29 | *10 | Balance of | 47 | 7.8 | |
| 30 | 20 | Balance of | 85 | 8.6 | |
| 31 | 30 | Balance of | 93 | 8.8 | |
| 32 | 40 | Balance of | 78 | 8.7 | |
| 33 | 50 | Balance of | 73 | 8.5 | |
| 34 | *60 | Balance of | 52 | 7.8 | |
| 35 | *80 | Balance of | 42 | 7.2 | |
| 36 | *100 | - | 39 | 6.5 | |
(values outside the scope of the invention are indicated by symbols)
As is clear from tables 1 to 4, the proportion of the spherical silver fine powder having an average particle diameter of 1.0 μm contained in the silver powder for silver clay is 15 to 50 mass% of silver clay 3 to 6, the proportion of the spherical silver fine powder having an average particle diameter of 1.5 μm contained in the silver powder for silver clay is 15 to 50 mass% of silver clay 12 to 15, and the proportion of the spherical silver fine powder having an average particle diameter of 0.5 μm contained in the silver powder for silver clay is 15 to 50 mass% of silver clay 21 to 24, and silver clay 30-33 containing spherical silver fine powder with an average particle diameter of 0.8 μm in a proportion of 15-50 mass% in the silver powder for silver clay, and a molded article obtained by molding the silver clay, the sintered body produced can obtain a considerably high tensile strength and density even if it is held at 600 c for 30 minutes, which is lower than usual. Therefore, it is clear that these silver clays are excellent in low-temperature sinterability.
Alternatively, if the spherical silver fine powder is contained outside the range of 15 to 50 mass%, sufficient tensile strength and density cannot be obtained. This is evident from the curve of fig. 2.
Example 5
30 mass% of spherical fine silver powder having an average particle diameter of 1.0 μm was mixed with an ultrafine silver powder having an average particle diameter of 5.0 μm to produce a silver powder for silver clay, and then methyl cellulose, a surfactant, olive oil and water were added to the obtained silver powder for silver clay in the proportions shown in Table 5 to produce silver clays 37 to 42.
These silver clays 37 to 42 were shaped and sintered at 600 ℃ for 30 minutes to produce a sintered body of a test piece having a thickness of 3mm, a width of 4mm and a length of 65mm, and the tensile strength and density of the obtained test piece were measured. The results are shown in Table 5.
| Species of | Composition ratio (mass%) | Characteristics of sintered body | ||||||
| Silver powder for silver clay | Methyl cellulose | Surface active agent | Olive oil | Water (W) | Tensile Strength (N/mm)2) | Density (g/cm)3) | ||
| Silver clay | 37 | (silver powder for silver clay comprising 30% of fine silver powder having an average particle diameter of 1.0 μm and the balance of ultrafine powder having an average particle diameter of 5 μm): 80 | 7.5 | - | - | Balance of | 90 | 8.2 |
| 38 | 3.0 | - | - | Balance of | 93 | 8.0 | ||
| 39 | 7.5 | 2.3 | - | Balance of | 100 | 8.7 | ||
| 40 | 4.5 | 1.0 | - | Balance of | 90 | 8.2 | ||
| 41 | 7.0 | - | 0.5 | Balance of | 95 | 8.3 | ||
| 42 | 5.5 | - | 1.3 | Balance of | 98 | 8.5 | ||
As can be seen from the results in table 5, the silver clay can obtain excellent low-temperature sinterability even if it does not contain any of the surfactant and the olive oil.
As described above, the silver clay according to the present invention can be sintered at a lower temperature than the silver clay of the prior art, can be used by more people, and can be easily manufactured into handicrafts, ornaments, etc., thereby exhibiting excellent effects.
Claims (10)
1. A silver powder for silver clay comprises a mixed powder of silver powder containing 15 to 50 mass% of fine silver powder having an average particle diameter of 2 μm or less and the balance of silver powder having an average particle diameter of more than 2 μm and 100 μm or less.
2. The silver powder for silver clay according to claim 1, which comprises a mixed powder comprising 15 to 50% by mass of fine silver powder having an average particle diameter of 0.5 to 1.5 μm and the balance of silver powder having an average particle diameter of 3 to 20 μm.
3. A silver clay comprising 50 to 95 mass% of the silver powder for silver clay according to claim 1, 0.8 to 8 mass% of an organic binder, and the balance being water.
4. A silver clay comprising 50 to 95 mass% of the silver powder for silver clay according to claim 2, 0.8 to 8 mass% of an organic binder, and the balance being water.
5. The silver clay according to claim 3, further comprising 0.03 to 3% by mass of a surfactant.
6. The silver clay according to claim 4, further comprising 0.03 to 3% by mass of a surfactant.
7. The silver clay according to claim 3, further comprising 0.1 to 3% by mass of an oil or fat.
8. The silver clay according to claim 4, further comprising 0.1 to 3% by mass of an oil or fat.
9. The silver clay according to claim 5, further comprising 0.1 to 3% by mass of an oil or fat.
10. The silver clay according to claim 6, further comprising 0.1 to 3% by mass of an oil or fat.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP301375/2001 | 2001-09-28 | ||
| JP2001301375A JP4265127B2 (en) | 2000-12-12 | 2001-09-28 | Silver powder for silver clay excellent in low temperature sintering property and silver clay containing this silver powder |
| PCT/JP2002/006064 WO2003028927A1 (en) | 2001-09-28 | 2002-06-18 | Silver powder for silver clay and silver clay comprising the silver powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| HK1071325A1 HK1071325A1 (en) | 2005-07-15 |
| HK1071325B true HK1071325B (en) | 2007-03-30 |
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