CN1313642C - Molten gold resisting high-temp sinter and its preparing process - Google Patents
Molten gold resisting high-temp sinter and its preparing process Download PDFInfo
- Publication number
- CN1313642C CN1313642C CNB01134072XA CN01134072A CN1313642C CN 1313642 C CN1313642 C CN 1313642C CN B01134072X A CNB01134072X A CN B01134072XA CN 01134072 A CN01134072 A CN 01134072A CN 1313642 C CN1313642 C CN 1313642C
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- CN
- China
- Prior art keywords
- gold
- resinate
- bismuth
- antimony
- thorium
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/5116—Ag or Au
Abstract
The present invention provides high-temperature resistant sintering liquid gold and a producing method thereof, which relates to ceramic decoration paint and a producing method thereof. The present invention is characterized in that the liquid gold comprises the components of the following proportion: 10 to 15 wt% of gold, 2.2 to 3.0 wt% of thorium, 0.1 to 0.3 wt% of rhodium, 0.1 to 0.8 wt% of antimony, 0.3 to 0.4 wt% of lead, 1.0 to 1.4 wt% of bismuth and a mixed solvent accounted for the rest weight. In the producing method, thorium nitrate, rhodium trichloride and antimony trichloride are respectively produced into resinate, and three kinds of the resinate are mixed to obtain additives of high temperature resistance liquid gold; after being produced into high gold ammonium chloride, gold trichloride reacts with sulfurization balsam to obtain a resinate gold solid body; lead nitrate and bismuth nitrate are respectively produced into resinate, and a liquid gold adhesive force reinforcing agent is obtained by uniformly mixing the lead nitrate with the bismuth nitrate; the additives of high temperature resistance liquid gold, the resinate gold solid body and the liquid gold adhesive force reinforcing agent, which are produced by the producing method, are mixed and finally diluted by the mixed solvent.
Description
One, technical field
The present invention relates to molten gold resisting high-temp sinter and preparation method thereof, belong to the technical field of ceramic decoration coating material production.
Two, background technology
Bright liquid gold is in Jinsui River again, is a kind of proof gold 10～12% that contains, and is added with the compound of metals such as a small amount of rhodium, chromium, bismuth, the brownish black thick liquid in oil medium.It can impose on the Ceramic glaze with modes such as brushing, stamps, and with weak fire heating (about 300 ℃), oil is evaporated and burns then, and gold-containing compound decomposes and leaves over down jewelly gold as thin as a wafer layer, can be bonded on the glaze securely during reheat to 750 ℃.Doing to decorate on the ceramic glaze with Jinsui River is one of cheap and good-quality gold trailing.Before the present invention, Jinsui River generally makes by following technology: gold is dissolved in chloroazotic acid obtains hydrochloro-auric acid, preparation sulfuration face cream and ammoniumper chlorate gold; Prepare golden organic compound; Preparation resinous acid chromium, bismuth resinate, resinous acid rhodium and ester (solvent); Prepare Jinsui River of necessary denseness (concentration).The subject matter that exists is that high temperature sintering resistant and sticking power are relatively poor, in Jinsui River of various prescriptions, the product that can high temperature resistant sintering reaches more than 850 ℃ is arranged seldom.There are gold and the sintering temperature contacted ceramic of people should be high more good more and decorate, so that the harmful material of some in the ceramic substrate material (as lead etc.) can in high-temperature sintering process, remove.Along with the relieving of national gold policy, the consumption of gold in ceramic decoration is increasing, so Jinsui River that R and D have a high temperature resistant sintering character has very big realistic meaning for ceramic decoration.
Three, summary of the invention
1, goal of the invention: the purpose of this invention is to provide a kind of molten gold resisting high-temp sinter and production method thereof with resistance to elevated temperatures and strong adhesion.
2, technology contents: a kind of molten gold resisting high-temp sinter, the components by weight percent in this Jinsui River are gold 5～10%, thorium 2.2～3.0%, rhodium 0.1～0.3%, antimony 0.1～0.8%, lead 0.3～0.4%, bismuth 1.0～1.4%, and all the other are mixed solvent; It is characterized in that described mixed solvent is is that 2～9% chloroform, 1～8% oil of mirbane mix by the turps of weight 24%, 41% star aniseed oil, 25% dibutyl phthalate and surplus.
The method of its preparation is at first making resinate respectively with thorium nitrate 99.99004323A8urity, Trichlororhodium, butter of antimony, above-mentioned three kinds of resinates are mixed, the weight content that makes thorium in the mixture is 5～10%, the weight content of rhodium is 0.5～1.0%, the weight content of antimony is 0.6～1.8%, obtains high temperature resistant Jinsui River additive; After gold perchloride made high gold trichloride ammonium, obtaining weight Gold Content with the reaction of sulfuration face cream was 50～65% resinous acid gold solid; Lead nitrate and Bismuth trinitrate are made resinate respectively, the two is mixed, making content plumbous in this mixture is 3.0%～5.0%, and the content of bismuth is 11.0%～17.0%, obtains Jinsui River sticking power toughener; High temperature resistant Jinsui River additive, resinous acid gold solid and Jinsui River sticking power toughener that above three parts are made mix, and dilute with mixed solvent at last.
3, positively effect: the fusing point of gold is 1064.43 ℃, and chemical property is very stable, is unique metal that does not at high temperature react with oxygen.And the decomposition temperature of the organic compound of gold is generally lower, gold is made organic compound, and to be applied to largest benefit on the ceramic surface again be that the distribution of gold is more even, and can form alloy in sintering process with other metal (must make organic compound in advance).Therefore, technological thought of the present invention is: in the suitable organic compound of gold, adding can form the organic compound of other metal of high temperature alloy with gold, under the prerequisite of the color effects that does not influence golden surface decoration, improve the high temperature resistant sintering character in Jinsui River, difference according to ceramic substrate material adds the different frit that can improve surface decoration gold sticking power simultaneously, thereby reaches the high temperature resistant sintering in raising Jinsui River and the purpose of sticking power.
Four, specific embodiments
1, in distilling flask, adds turps, collect 165～170 ℃ of cuts.The turps cut that obtains is added in another distilling flask, add the sulphur powder, the quality percentage composition that makes the sulphur powder is 8-10%, be heated to 160 ℃ and be incubated 4 hours, continue heating, distillation is when the volume of distillate reaches turps volume about 25% time of adding, stop distillation, regulating the sulphur content of staying the sulfuration face cream in the flask with new distillatory turps is 10-12%.
2, the electrolysis bronze is dissolved in chloroazotic acid, removes the redundant nitric acid postcooling.The ratio of down payment/ammonium chloride under constantly stirring=1: 0.3 adds ammonium chloride, and heating in water bath obtains ammoniumper chlorate gold solid to doing.Down payment: the ratio of dehydrated alcohol=1: 5 adds dehydrated alcohol, and ammoniumper chlorate gold solid is dissolved fully.Down payment: the ratio of sulfuration face cream=1: 3.5 dropwise adds sulfuration face cream (adding in 1-1.5 hour).Stop heating at this miscellany of heating on the boiling water bath after 1.5 hours.Add a small amount of dehydrated alcohol and thoroughly stirring, leave standstill, with decantation resinous acid gold solid is inclined to, and become powdery solid with absolute ethanol washing to resinous acid gold.Filter, with the gained pressed powder in 40 ℃ of following vacuum-dryings.
3, press RhCl
3: the ratio of dehydrated alcohol=1: 10, Trichlororhodium is dissolved in the dehydrated alcohol, filter; Press RhCl
3: the ratio of sulfuration face cream=1: 5, in filtrate, add the sulfuration face cream, fully after the reaction, with dehydrated alcohol with the washing of precipitate of resinous acid rhodium to there not being Cl
-Till.Filter, the gained pressed powder in 40 ℃ of following vacuum-dryings, is made the resinous acid rhodium.
4, by preparing the same method of resinous acid rhodium lead nitrate, Bismuth trinitrate, thorium nitrate 99.99004323A8urity and butter of antimony are made corresponding resinate.
5, mixed solvent: new distillatory turps (24%), star aniseed oil (41%), dibutyl phthalate (25%), chloroform (2～9%), oil of mirbane (1～8%) are made into mixed solvent.
6, take by weighing a certain amount of resinous acid gold, resinous acid rhodium, resinous acid antimony, resinous acid thorium, lead resinate and bismuth resinate, be dissolved in the mixed solvent respectively at heating in water bath with under stirring.With resinous acid thorium, resinous acid rhodium and three kinds of resinous acid salt solution mix of resinous acid antimony, make the content of thorium in the mixture, rhodium and antimony be in 5～10%, 0.5～1.0% and 0.6～1.8% respectively, obtain high temperature resistant Jinsui River additive.Lead resinate and bismuth resinate solution are mixed, and content plumbous and bismuth is respectively 4.0%+1 and 14.0+3% in the mixture, obtains Jinsui River sticking power toughener.
7, above-mentioned resinous acid gold solution, high temperature resistant Jinsui River additive and Jinsui River sticking power toughener are mixed, the content of gained gold underwater gold, thorium, rhodium, antimony, lead, bismuth is in respectively between 10～15%, 2.2～3.0%, 0.1～0.3%, 0.1～0.8%, 0.3～0.4%, 1.0～1.4%.Obtain molten gold resisting high-temp sinter.The content of adjusting thorium, rhodium, antimony in Jinsui River can get high temperature resistant sintering Jinsui River 860-980 ℃ of scope.
Embodiment 1: add 20g electrolysis bronze in Florence flask, add chloroazotic acid 100mL, heating in water bath all dissolves until bronze.Add small amount of hydrochloric acid and continue heating to remove redundant nitric acid.Cooling is filtered.The 6g chloride solid is dissolved in less water, under constantly stirring ammonium chloride solution is joined and contain in the golden filtrate, heating in water bath obtains ammoniumper chlorate gold solid to doing.Ammoniumper chlorate gold solid is dissolved in the 100mL dehydrated alcohol, dropwise adds 70g sulfuration face cream (adding in 1～1.5 hour).Stop heating at this miscellany of heating on the boiling water bath after 1.5 hours.Add a small amount of dehydrated alcohol and thoroughly stirring, leave standstill, with decantation resinous acid gold solid is inclined to, and become powdery solid with absolute ethanol washing to resinous acid gold.Filter, with the gained pressed powder in 40 ℃ of following vacuum-dryings.
Get 2g Trichlororhodium, 50g thorium nitrate 99.99004323A8urity, 100g lead nitrate, 100g Bismuth trinitrate and 50g butter of antimony and be dissolved in respectively in the dehydrated alcohol, produce resinous acid rhodium, resinous acid thorium, lead resinate, bismuth resinate and resinous acid antimony respectively by preceding method.Resinous acid rhodium, resinous acid thorium, lead resinate, bismuth resinate and the resinous acid antimony of gained are dissolved in respectively in the mixed solvent, are made into the resinous acid thorium solution of resinous acid rhodium solution, the thoriated 20% of rhodium-containing 5%, the resinous acid antimony solution that contains antimony 10%, leaded 10% lead resinate solution and the bismuth resinate solution of bismuth-containing 30%.
Take by weighing resinous acid rhodium solution 20.0g, the thoriated 20% of rhodium-containing 5.0% resinous acid thorium solution 50.0g, contain the resinous acid antimony solution 18.0g and the mixed solvent 12.0g of antimony 10%, mix, obtain high temperature resistant Jinsui River additive (content of thorium, rhodium, antimony is respectively 10.0%, 1.0% and 1.8%).Accurately take by weighing leaded 10% lead resinate solution 40g, the bismuth resinate solution 46.7g and the mixed solvent 13.3g of bismuth-containing 30%, mix, obtain Jinsui River sticking power toughener (content plumbous and bismuth is respectively 4.0% and 14.0%).
Get 10g resinous acid gold solid and be dissolved in the 20g mixed solvent, add 15g high temperature resistant Jinsui River additive and 5g sticking power toughener, mix, obtain sample No. 1.Hardened coating on white glaze, high temperature sintering test, high-temperature resistant can reach 980 ℃, the golden film on this sintering temperature resulting product surface, any surface finish, leakless, golden film and substrate caking power reach 950g/mm
2
Embodiment 2: the same quadrat method by embodiment 1 prepares resinous acid gold, resinous acid thorium, resinous acid rhodium, resinous acid antimony, lead resinate and bismuth resinate, and the resinous acid thorium solution of resinous acid rhodium solution, the thoriated 20% of preparation rhodium-containing 5%, the resinous acid antimony solution that contains antimony 10%, leaded 10% lead resinate solution and the bismuth resinate solution of bismuth-containing 30%.Accurately take by weighing resinous acid rhodium solution 10.0g, the thoriated 20% of rhodium-containing 5.0% resinous acid thorium solution 25.0g, contain the resinous acid antimony solution 6.0g and the mixed solvent 59.0g of antimony 10%, mix, obtain high temperature resistant Jinsui River additive (content of thorium, rhodium, antimony is respectively 5.0%, 0.5% and 0.6%).Accurately take by weighing leaded 10% lead resinate solution 40g, the bismuth resinate solution 46.7g and the mixed solvent 13.3g of bismuth-containing 30%, mix, obtain Jinsui River sticking power toughener (content plumbous and bismuth is respectively 4.0% and 14.0%).
Get 10g resinous acid gold solid and be dissolved in the 20g mixed solvent, add 15g high temperature resistant Jinsui River additive and 5g sticking power toughener, mix, obtain sample No. 2.Hardened coating on white glaze, high temperature sintering test, high-temperature resistant can reach 860 ℃.
Embodiment 3: the same quadrat method by embodiment 1 prepares resinous acid gold, resinous acid thorium, resinous acid rhodium, resinous acid antimony, lead resinate and bismuth resinate, and the resinous acid thorium solution of resinous acid rhodium solution, the thoriated 20% of preparation rhodium-containing 5%, the resinous acid antimony solution that contains antimony 10%, leaded 10% lead resinate solution and the bismuth resinate solution of bismuth-containing 30%.Accurately take by weighing resinous acid rhodium solution 15.0g, the thoriated 20% of rhodium-containing 5.0% resinous acid thorium solution 40.0g, contain the resinous acid antimony solution 12.0g and the mixed solvent 43.0g of antimony 10%, mix, obtain high temperature resistant Jinsui River additive (content of thorium, rhodium, antimony is respectively 8.0%, 0.75% and 1.2%).Accurately take by weighing leaded 10% lead resinate solution 40g, the bismuth resinate solution 46.7g and the mixed solvent 13.3g of bismuth-containing 30%, mix, obtain Jinsui River sticking power toughener (content plumbous and bismuth is respectively 4.0% and 14.0%).
Get 10g resinous acid gold solid and be dissolved in the 20g mixed solvent, add 15g high temperature resistant Jinsui River additive and 5g sticking power toughener, mix, obtain sample No. 3.Hardened coating on white glaze, high temperature sintering test, high-temperature resistant can reach 910 ℃.
Claims (2)
1, a kind of molten gold resisting high-temp sinter, the components by weight percent in this Jinsui River are gold 5～10%, thorium 2.2～3.0%, rhodium 0.1～0.3%, antimony 0.1～0.8%, lead 0.3～0.4%, bismuth 1.0～1.4%, and all the other are mixed solvent; It is characterized in that described mixed solvent is is that 24% turps, 41% star aniseed oil, 25% dibutyl phthalate and surplus are that 2～9% chloroform, 1～8% oil of mirbane mix by weight.
2, a kind of production method of molten gold resisting high-temp sinter, it is characterized in that at first thorium nitrate 99.99004323A8urity, Trichlororhodium, butter of antimony being made resinate respectively, above-mentioned three kinds of resinates are mixed, the weight content that makes thorium in the mixture is 5～10%, the weight content of rhodium is 0.5～1.0%, the weight content of antimony is 0.6～1.8%, obtains high temperature resistant Jinsui River additive; After gold perchloride made high gold trichloride ammonium, obtaining weight Gold Content with the reaction of sulfuration face cream was 50～65% resinous acid gold solid; Lead nitrate and Bismuth trinitrate are made resinate respectively, the two is mixed, making content plumbous in this mixture is 3.0%～5.0%, and the content of bismuth is 11.0%～17.0%, obtains Jinsui River sticking power toughener; High temperature resistant Jinsui River additive, resinous acid gold solid and Jinsui River sticking power toughener that above three parts are made mix, and dilute with mixed solvent at last.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB01134072XA CN1313642C (en) | 2001-10-23 | 2001-10-23 | Molten gold resisting high-temp sinter and its preparing process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB01134072XA CN1313642C (en) | 2001-10-23 | 2001-10-23 | Molten gold resisting high-temp sinter and its preparing process |
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| Publication Number | Publication Date |
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| CN1363723A CN1363723A (en) | 2002-08-14 |
| CN1313642C true CN1313642C (en) | 2007-05-02 |
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| CNB01134072XA Expired - Fee Related CN1313642C (en) | 2001-10-23 | 2001-10-23 | Molten gold resisting high-temp sinter and its preparing process |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100488918C (en) * | 2006-04-28 | 2009-05-20 | 冯建光 | Method for preparing imitating gold water |
| GB0905894D0 (en) * | 2009-04-06 | 2009-05-20 | Univ Belfast | Ionic liquids solvents for metals and metal compounds |
| JP5415628B2 (en) * | 2010-12-07 | 2014-02-12 | ルビコン株式会社 | Capacitor, capacitor case and circuit board |
| CN103387419B (en) * | 2013-08-21 | 2017-04-05 | 景德镇市欧格陶瓷有限公司 | A kind of porcelain Jinsui River and its using method suitable for microwave oven |
| JP6780039B2 (en) | 2019-01-25 | 2020-11-04 | 株式会社ノリタケカンパニーリミテド | Water gold liquid for inkjet |
| CN110453203A (en) * | 2019-08-13 | 2019-11-15 | 北京科技大学 | A kind of organic chemistry additive and its application method for gold paste material |
| CN112735631B (en) * | 2020-12-21 | 2022-10-21 | 有研工程技术研究院有限公司 | Low-viscosity organic gold paste capable of being sintered on surface of circuit board substrate at low temperature |
| CN113921165B (en) * | 2021-12-14 | 2022-03-29 | 西安宏星电子浆料科技股份有限公司 | Organic gold slurry |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1060483A (en) * | 1990-09-14 | 1992-04-22 | 日本金液株式会社 | The overglaze color composition that contains precious metal that is used for pottery |
| CN1069995A (en) * | 1991-08-30 | 1993-03-17 | 唐山市陶瓷工业公司研究所 | Bright orange Jinsui River of no rhodium and preparation method |
| CN1072670A (en) * | 1992-11-15 | 1993-06-02 | 山东省硅酸盐研究设计院 | Jinsui River |
-
2001
- 2001-10-23 CN CNB01134072XA patent/CN1313642C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1060483A (en) * | 1990-09-14 | 1992-04-22 | 日本金液株式会社 | The overglaze color composition that contains precious metal that is used for pottery |
| CN1069995A (en) * | 1991-08-30 | 1993-03-17 | 唐山市陶瓷工业公司研究所 | Bright orange Jinsui River of no rhodium and preparation method |
| CN1072670A (en) * | 1992-11-15 | 1993-06-02 | 山东省硅酸盐研究设计院 | Jinsui River |
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