CN111044179B - Method for manufacturing fixed point furnace gold fixed point bottle - Google Patents
Method for manufacturing fixed point furnace gold fixed point bottle Download PDFInfo
- Publication number
- CN111044179B CN111044179B CN201911234075.5A CN201911234075A CN111044179B CN 111044179 B CN111044179 B CN 111044179B CN 201911234075 A CN201911234075 A CN 201911234075A CN 111044179 B CN111044179 B CN 111044179B
- Authority
- CN
- China
- Prior art keywords
- bottle
- fixed
- gold
- point
- purity
- Prior art date
- 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.)
- Active
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K15/00—Testing or calibrating of thermometers
- G01K15/005—Calibration
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/02—Sealings between relatively-stationary surfaces
- F16J15/06—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces
- F16J15/062—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces characterised by the geometry of the seat
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/02—Sealings between relatively-stationary surfaces
- F16J15/06—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces
- F16J15/10—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with non-metallic packing
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
- F27B17/02—Furnaces of a kind not covered by any preceding group specially designed for laboratory use
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D21/00—Arrangements of monitoring devices; Arrangements of safety devices
- F27D21/0014—Devices for monitoring temperature
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/02—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using thermoelectric elements, e.g. thermocouples
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
- F27D2007/063—Special atmospheres, e.g. high pressure atmospheres
Abstract
The invention discloses a method for manufacturing a fixed point furnace gold fixed point bottle, which comprises the following steps: adding a first batch of high-purity gold raw material into a quartz bottle; vacuumizing the quartz bottle to set conditions, and filling argon; placing the quartz bottle in a fixed-point furnace for heating and melting; stopping heating and completely cooling after the high-purity gold raw material is completely melted; adding a second batch of high-purity gold raw materials into the quartz bottle, repeating the steps, completely melting all the high-purity molten gold raw materials, and cooling; heating by a fixed-point furnace to obtain a melting temperature plateau of the high-purity gold; cooling by a fixed-point furnace to obtain a solidified temperature plateau of the high-purity gold; comparing the melting point of the melting temperature plateau and the solidifying temperature plateau with the melting point of 1064.18 ℃ of high-purity gold, and adjusting the Ar gas pressure in a fixed point bottle to 1 standard atmospheric pressure; and finally, sealing the quartz bottle to finish the manufacture of the high-purity gold fixed point bottle. The invention provides a method for manufacturing a fixed point furnace gold fixed point bottle, which effectively prolongs the service life of the fixed point bottle used for temperature verification at 1000 ℃ and improves the calibration accuracy.
Description
Technical Field
The invention relates to the field of thermotechnical metering, in particular to a method for manufacturing a fixed point furnace gold fixed point bottle.
Background
In the fields of temperature measurement calibration and the like, the detection of the thermocouple is carried out by a comparison method in domestic general industrial production. The calibration of the thermoelectric voltage values of the R, S, B thermocouple was compared with the standard thermocouple at predetermined temperature points, which were typically three points of Zn, Al, and Cu (Au). Since the standard thermocouple has lower and lower measurement accuracy in the use process, with the development of scientific technology, more and more enterprises and measurement units start to use fixed points for calibration, which can eliminate the deviation caused by the standard thermocouple in the comparison method. When the fixed point is selected for detection, the international temperature scale ITS90 is at 1000 ℃, the temperature fixed points are defined as Cu (1084.62 ℃) and Au (1064.18 ℃), but all fixed point equipment suppliers on the market currently only provide fixed point bottles with Cu points. This is mainly due to the fact that the price difference between Au and Cu is too large, but since Cu is more easily oxidized than Au, the life of the Cu-fixed-point bottle is much shorter than that of the Au-fixed-point bottle.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the invention provides a method for manufacturing a fixed point furnace gold fixed point bottle, which solves the problems.
The invention is realized by the following technical scheme:
a method for manufacturing a fixed point furnace gold fixed point bottle comprises the following steps:
step 1, adding a first batch of high-purity gold raw material into a quartz bottle;
step 2, vacuumizing the interior of the quartz bottle, and filling argon into the quartz bottle after the vacuum degree of the interior of the quartz bottle reaches a set condition;
step 4, stopping heating after the first batch of high-purity gold raw materials added into the quartz bottle are completely melted, and completely cooling the melted high-purity gold;
step 5, adding a second batch of high-purity gold raw materials into the quartz bottle, repeating the step 1 to the step 4, completely melting all the high-purity melting gold raw materials in the quartz bottle, and cooling to finish the process;
step 6, heating the fixed-point furnace, melting the high-purity gold in the quartz bottle, and obtaining a melting temperature plateau of the high-purity gold; then cooling the fixed point furnace to cool the high-purity gold in the quartz bottle to obtain a solidification temperature plateau of the high-purity gold;
step 7, comparing the melting point 1064.18 ℃ of the melting temperature plateau and the solidifying temperature plateau with the melting point 1064.18 ℃ of the high-purity gold, and adjusting the Ar gas pressure in a fixed point bottle to 1 standard atmospheric pressure;
and 8, finally sealing the quartz bottle to finish the manufacture of the high-purity gold fixed point bottle.
Furthermore, the purity of the high-purity gold is more than or equal to 6N.
The purity of the high-purity gold needs to be more than 6N, namely the purity reaches more than 99.9999 percent; typically by purchasing raw materials from an outside supplier.
Further, the total weight of the high-purity gold raw material is 1 kg-3 kg; the shape of the high-purity gold raw material comprises granular, powdery and flaky shapes, and the granular high-purity gold with the diameter of 3 mm-5 mm is preferred.
The weight of the high-purity gold is determined to be 1kg to 3kg, and the preferred scheme is 2.5kg according to the volume of the gold fixed point bottle to be manufactured. The shape of the high-purity gold raw material comprises but is not limited to granules, powder, flakes and the like. Preferably, the gold is granular high-purity gold with the diameter of 3 mm-5 mm.
Further, in the step 2, the quartz bottle is vacuumized until the vacuum degree is less than 1Pa, and preferably less than or equal to 0.1 Pa; filling high-purity argon with 1 standard atmosphere, wherein the purity of the argon is more than or equal to 99.99 percent.
Furthermore, in the step 3, the heating and melting temperature is set to 1060 ℃, and then the temperature is raised to 1620 ℃ to continue heating and melting.
Further, in the step 4, a plurality of groups of thermocouples are adopted to monitor the gold dissolution condition in the quartz bottle in real time; the thermocouples are arranged in the quartz bottle and are distributed in sequence in the height direction of the quartz bottle in a set height gradient.
In order to monitor the melting condition of high-purity gold in real time, a plurality of groups of thermocouples, such as three groups of thermocouples, can be adopted, each group is placed in a quartz bottle by taking the height of 50-100 mm as a gradient, and the dissolution condition of the gold in a fixed-point bottle is observed by connecting a high-precision digital multimeter and through a potential value.
Further, in the step 6, the specific operation steps include:
step 61, measuring the temperature related information of the high-purity gold in the quartz bottle by adopting a thermocouple; setting the temperature of the fixed point furnace to 1060 ℃, and starting to measure the potential value of the thermocouple;
step 62, setting the temperature of the fixed-point furnace to be 1080 ℃, melting the high-purity gold in the quartz bottle, and obtaining a melting temperature plateau of the high-purity gold according to the measured value;
and step 63, setting the temperature of the fixed-point furnace to 1060 ℃, starting to reduce the temperature, and obtaining the solidification temperature plateau of the high-purity gold according to the measured value.
Furthermore, three standard S or R type thermocouples which are distributed in a step shape with equal height are inserted into the quartz bottle, and the temperature related information of the high-purity gold in the quartz bottle is measured.
A sealing protection sleeve comprises a lower assembly main body and an upper assembly main body which are mutually detachable, hermetically matched and annular, wherein the lower assembly main body and the upper assembly main body are sequentially sealed and sleeved at an upper port of a fixed point bottle from bottom to top; the upper assembly main body is provided with an air exhaust pipeline and an air inflation pipeline, the air exhaust pipeline is used for communicating the internal environment of the fixed point bottle with external air exhaust equipment, and the air inflation pipeline is used for communicating the fixed point bottle with external air inflation equipment; the sealing protective sleeve is used for vacuumizing and inflating in the manufacturing method of the fixed point furnace gold fixed point bottle.
The air pressure and atmosphere are important factors influencing the manufacture of the gold fixed point, so how to quickly and accurately control the air pressure in the fixed point bottle and replace the air with inert atmosphere has important significance for prolonging the service life and the accuracy of the gold fixed point bottle, shortening the manufacturing period and reducing the manufacturing cost. The sealing protective sleeve provided by the invention is used in the process of manufacturing a fixed bottle, is beneficial to realizing rapid air pressure adjustment and atmosphere replacement, and has the advantages of simple structure and convenience in disassembly and assembly. The sealing protection sleeve is of a main framework structure consisting of a lower assembly main body and an upper assembly main body which are of annular structures; the lower assembly main body is mainly used for fixing the quartz bottle, determining the height and performing sealing operation on the quartz bottle by matching with the upper assembly main body; go up the subassembly main part, its main function is with subassembly main part cooperation play the effect of sealing up whole quartz bottle down. After the quartz bottle is fixed and sealed by the upper assembly main body and the lower assembly main body, the upper assembly main body and the lower assembly main body are connected to a vacuum pump through an air exhaust pipeline to vacuumize the inside of the quartz bottle, and the lower assembly main body is connected to an inert gas argon bottle through an air inflation pipeline to fill argon into the quartz bottle.
Furthermore, a plurality of lower assembly bolt holes are formed in the lower assembly main body and are uniformly distributed along the circumferential direction of the lower assembly main body; the upper assembly main body is provided with a plurality of upper assembly bolt holes which are uniformly distributed along the circumferential direction of the upper assembly main body; the bolt sequentially penetrates through the upper assembly bolt hole and the corresponding lower assembly bolt hole to realize that the upper assembly main body and the lower assembly main body are detachably connected.
Go up the subassembly main part and pass through the bolt detachable connection with subassembly main part down, simple structure is convenient for to whole sealed protection sleeve dismouting operation.
Further, the lower assembly main body further comprises a lower assembly O-shaped sealing ring, and the upper assembly main body further comprises an upper assembly O-shaped sealing ring; the lower component O-shaped sealing ring and the upper component O-shaped sealing ring are sleeved on the outer wall of the port of the fixed point bottle, and the lower component O-shaped sealing ring and the upper component O-shaped sealing ring are compressed and fixed between the upper component main body and the lower component main body and are in sealing contact with the outer wall of the fixed point bottle.
On one hand, the lower component O-shaped sealing ring and the upper component O-shaped sealing ring are compressed between the upper component main body and the lower component main body, and play a role in sealing the contact part between the upper component main body and the lower component main body; on the other hand, the inner walls of the lower component O-shaped sealing ring and the upper component O-shaped sealing ring are in close contact with the outer wall of the top port of the quartz bottle, so that the quartz bottle is sealed.
Furthermore, a sealing cover is arranged on the upper assembly main body and covers the top port of the annular structure of the upper assembly main body in a sealing manner; the sealing cover is provided with a through hole for communicating the air exhaust pipeline and the air inflation pipeline with the fixed point bottle.
Through setting up sealed lid, its main effect is for can adding high-purity gold raw materials in the quartz bottle under the sealed protective sheath spare condition of not dismantling.
Furthermore, a lower assembly cooling cavity which is continuously distributed along the annular direction is arranged in the lower assembly main body, and a coolant is introduced into the lower assembly cooling cavity through a lower assembly cooling pipeline; the upper assembly cooling cavity is arranged in the upper assembly main body and continuously distributed along the annular direction, and a coolant is guided into the lower assembly cooling cavity through an upper assembly cooling pipeline.
Through setting up the cooling line, do benefit to the sealed protective sheath spare that ensures the quartz bottle bottleneck and set up and do not receive high temperature to influence life, do benefit to especially that the last subassembly O type sealing washer that protects the rubber system and lower subassembly O type sealing washer is not melted by the heat that the gold melts the production in use.
The invention has the following advantages and beneficial effects:
1. the invention provides a method for manufacturing a fixed point furnace gold fixed point bottle, which effectively prolongs the service life of the fixed point bottle used for temperature verification at 1000 ℃ and improves the calibration accuracy, and the manufactured high-purity gold fixed point bottle has the uncertainty of less than 8mK and K is 2, so that the fixed point bottle is manufactured by high-purity gold to replace the existing Cu metal fixed point bottle;
2. the invention provides a sealing protective sleeve which is used in a manufacturing method of a gold fixed point bottle, can realize the purposes of quickly and accurately vacuumizing and inflating for replacing air, has a simple structure, is convenient to disassemble, is beneficial to processing and storing, and is beneficial to preparing a high-precision high-purity gold fixed point bottle.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a fixed point bottle protecting jacket for high purity gold according to the present invention; wherein, (a) represents a schematic top view structure; (b) a schematic diagram showing a main view structure;
fig. 2 is a schematic view of the assembly of the gold anchor point bottle and the protective sleeve of the present invention.
Reference numbers and corresponding part names in the drawings: the sealing structure comprises a lower component main body, a lower component O-shaped sealing ring, a lower component cooling water pipeline, a lower component bolt hole, an upper component main body, an upper component O-shaped sealing ring, an upper component cooling water pipeline, an upper component bolt hole, and a sealing cover of the upper component.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1
The embodiment provides a method for manufacturing a fixed point furnace gold fixed point bottle, which comprises the following specific steps:
step 1, preparing a high-purity gold raw material, wherein the purity of the high-purity gold is required to be more than 6N, namely the purity is more than 99.9999%. Typically by purchasing raw materials from an outside supplier. The weight of the high-purity gold is determined to be 2.5kg according to the volume of the gold fixed point bottle to be manufactured, granular high-purity gold with the diameter of 5mm is adopted, and the high-purity gold raw material is melted in the quartz bottle in batches.
And 2, preparing a high-purity quartz bottle for containing high-purity gold, wherein the bottom end of the quartz bottle is closed, and the top end of the quartz bottle is opened. The size of the quartz bottle is matched with the hearth of the corresponding fixed point holding furnace. The preferred size of the quartz bottle is 620mm, or is the standard empty quartz bottle provided by the fixed point holding furnace manufacturer. Meanwhile, in order to mount the seal protector more favorably, a 150mm portion of the upper portion of the quartz bottle needs to be sandblasted to roughen the surface.
And 3, firstly, adding a first batch of high-purity gold raw material into a quartz bottle, and filling about 500g of high-purity gold particles into the first batch according to the proportion.
Step 4, vacuumizing the interior of the quartz bottle, and filling argon into the quartz bottle after the vacuum degree of the interior of the quartz bottle reaches a set condition; vacuumizing the quartz bottle to 0.1 Pa; filling high-purity argon with the purity of more than or equal to 99.99 percent to keep the pressure in the quartz bottle at 1 standard atmospheric pressure.
And 5, placing the prepared quartz bottle into a fixed point furnace, and setting the temperature to 1060 ℃. And simultaneously heating the gold particles in the bottle to be spotted.
Step 6, preparing three groups of standard thermocouples for monitoring the melting condition of gold in real time, wherein each group is placed in a quartz bottle with the height of 50-100 mm as a gradient, and preferably, each group is placed in the quartz bottle after being bundled with the height of 75mm as the gradient; then, a high-precision Fluke8050A digital multimeter is connected to the mv grade, and the melting condition of the high-purity gold in the quartz bottle is observed through the potential value. Adjusting the furnace temperature of the fixed point furnace to 1620 ℃, and completely melting the high-purity gold in the quartz bottle. Meanwhile, in the period, the air pumping and the air inflation are required to be carried out continuously, and all air in the quartz bottle and the high-purity gold liquid is replaced by argon (Ar). And after the first batch of high-purity gold in the quartz bottle is completely melted, namely after the potential value of the lowest thermocouple begins to rise, closing the fixed-point furnace to completely cool the fixed-point furnace.
Step 7, adding a second batch of high-purity gold raw materials into the quartz bottle, repeating the steps 3-6 until the last batch of high-purity melting gold raw materials are completely melted in the quartz bottle, and entering the step 8 after cooling is completed;
step 8, inserting three qualified standard S, R thermocouples which are bound in a step-like manner with equal height into the quartz bottle, preferably an R-type thermocouple in the embodiment, and the height gradient between adjacent thermocouples is 75mm, and then sequentially performing the following operations:
(1) setting the temperature of the fixed point furnace to 1060 ℃, and starting to measure the potential value of the thermocouple;
(2) setting the temperature of a fixed point furnace to be 1080 ℃, melting the high-purity gold in the quartz bottle, and obtaining a melting temperature plateau of the high-purity gold according to a measured value;
(3) setting the temperature of the fixed-point furnace to 1060 ℃, starting to reduce the temperature, and obtaining the solidification temperature plateau of the high-purity gold according to the measured value.
Step 9, comparing the melting point 1064.18 ℃ of the melting temperature plateau and the solidifying temperature plateau with the melting point 1064.18 ℃ of the high-purity gold, and adjusting the Ar gas pressure in a fixed point bottle to 1 standard atmospheric pressure;
and step 10, finally sealing the quartz bottle to finish the manufacture of the high-purity gold fixed point bottle.
Example 2
The embodiment provides a sealed protection sleeve, including the lower subassembly main part 1 and the last subassembly main part 5 of mutually can dismantling sealed adaptation, lower subassembly main part 1 and last subassembly main part 5 all adopt ring annular structure, and establish the upper portion port department at the fixed point bottle by supreme seal cover in proper order down. 4-8 lower assembly bolt holes 4 are formed in the lower assembly main body 1, and all the lower assembly bolt holes 4 are uniformly distributed along the annular direction of the lower assembly main body 1 at equal intervals; 4-8 upper assembly bolt holes 8 are formed in the upper assembly main body 5, and all the upper assembly bolt holes 8 are uniformly distributed along the annular direction of the upper assembly main body 5 at equal intervals; the upper assembly main body 5 and the lower assembly main body 1 are detachably connected by sequentially penetrating through the upper assembly bolt hole 8 and the corresponding lower assembly bolt hole 4 through bolts. The lower assembly main body 1 further comprises a lower assembly O-shaped sealing ring 2, and the upper assembly main body 5 further comprises an upper assembly O-shaped sealing ring 6; lower subassembly O type sealing washer 2 and last subassembly O type sealing washer 6 all overlap and establish fixed point bottle port outer wall department, and lower subassembly O type sealing washer 2 and last subassembly O type sealing washer 6 compress tightly to be fixed between last subassembly main part 5 and lower subassembly main part 1, and all with fixed point bottle outer wall sealing contact. The upper assembly main body 5 is provided with an air exhaust pipeline 10 and an air inflation pipeline 11, the air exhaust pipeline 10 is used for communicating the internal environment of the fixed point bottle with external air exhaust equipment, and the air inflation pipeline is used for communicating the fixed point bottle with external air inflation equipment; the upper assembly main body 5 is provided with a sealing cover 9, and the sealing cover 9 is covered on the top port of the annular structure of the upper assembly main body 5 in a sealing way; the sealing cover 9 is provided with a through hole for communicating the air exhaust pipeline 10 and the air inflation pipeline 11 with the fixed point bottle. The inner diameter of the air exhaust pipeline 10 is selected to be phi 4-phi 8mm, the wall thickness is 0.75-1.5 mm, preferably the inner diameter is phi 6mm, the wall thickness is 1mm, the material is selected to be a steel pipe, and preferably 304 stainless steel. The inner diameter of the inflation pipeline 11 is selected to be phi 4-phi 8mm, the wall thickness is 0.75-1.5 mm, preferably the inner diameter phi 6mm, the wall thickness is 1mm, the material is selected to be a steel pipe, and preferably 304 stainless steel.
In addition, a lower assembly cooling chamber which is continuously distributed along the annular direction is arranged in the lower assembly main body 1, a coolant is introduced into the lower assembly cooling chamber through a lower assembly cooling pipeline 3, the inner diameter of a pipeline of the lower assembly cooling pipeline 3 is selected to be phi 4-phi 8mm, the wall thickness is 0.75-1.5 mm, preferably the inner diameter phi 6mm, the wall thickness is 1mm, and a steel pipe is selected as a material, preferably 304 stainless steel; an upper assembly cooling chamber which is continuously distributed along the annular direction is arranged in the upper assembly main body 5, and a coolant is introduced into the lower assembly cooling chamber through an upper assembly cooling pipeline 7; the pipe diameter of the upper assembly cooling pipeline 7 is selected to be phi 4-phi 8mm, and the wall thickness is 0.75-1.5 mm. The material is selected from steel pipe, preferably 304 stainless steel.
The sealing protection sleeve is used in embodiment 1, and has the functions of simply exhausting, inflating and charging the fixed-point bottle, and a corresponding cooling water path needs to be designed in the sealing protection member to ensure that a rubber sealing ring in the sealing protection member is not melted by heat generated by melting gold in use.
Install sealed protective sheath spare on the quartz bottle, take out the experiment of aerifing: connecting the free end of the air exhaust pipeline 10 with a pressure gauge, wherein the pressure gauge is connected with a valve, and the rear end of the valve is connected with a joint on a vacuum pump set; the free end of the gas-filled line 11 is connected to a cylinder of high purity argon via a closable valve. Vacuumizing the quartz bottle to 0.1Pa, then closing the vacuum pump, and determining whether the air leakage condition occurs; if no gas leakage occurs, a gas filling experiment is carried out, and high-purity argon gas is filled into a quartz bottle, so that the pressure in the quartz bottle is kept at 1 atmosphere of 101.325 KPa. In addition, when adding high-purity gold principle, only need open the sealed lid of sealed protection sleeve spare, add in batches not melt high-purity gold particle can, need not to dismantle whole sealed protection sleeve spare, the simple operation.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (13)
1. The manufacturing method of the fixed point furnace gold bottle is characterized by comprising the following steps:
step 1, adding a first batch of high-purity gold raw material into a quartz bottle;
step 2, vacuumizing the interior of the quartz bottle, and filling argon into the quartz bottle after the vacuum degree of the interior of the quartz bottle reaches a set condition;
step 3, placing the inflated quartz bottle in a fixed-point furnace for heating, and heating and melting;
step 4, stopping heating after the first batch of high-purity gold raw materials added into the quartz bottle are completely melted, and completely cooling the melted high-purity gold;
step 5, adding a second batch of high-purity gold raw materials into the quartz bottle, repeating the step 1 to the step 4, completely melting all the high-purity melting gold raw materials in the quartz bottle, and cooling to finish the process;
step 6, heating the fixed-point furnace, melting the high-purity gold in the quartz bottle, and obtaining a melting temperature plateau of the high-purity gold; then cooling the fixed point furnace to cool the high-purity gold in the quartz bottle to obtain a solidification temperature plateau of the high-purity gold;
step 7, comparing the melting point 1064.18 ℃ of the melting temperature plateau and the solidifying temperature plateau with the melting point 1064.18 ℃ of the high-purity gold, and adjusting the Ar gas pressure in a fixed point bottle to 1 standard atmospheric pressure;
step 8, finally sealing the quartz bottle to finish the manufacture of the high-purity gold fixed point bottle;
in the step 3, firstly, the heating and melting temperature is set to 1060 ℃, and then the temperature is raised to 1620 ℃ for continuous heating and melting;
in the step 4, a plurality of groups of thermocouples are adopted to monitor the gold dissolution condition in the quartz bottle in real time; the thermocouples are arranged in the quartz bottle and are distributed in sequence in the height direction of the quartz bottle in a set height gradient.
2. The method for manufacturing the fixed-point furnace gold fixed-point bottle according to claim 1, wherein the purity of the high-purity gold is more than or equal to 6N.
3. The method for manufacturing the fixed point furnace gold fixed point bottle according to claim 2, wherein the total weight of the high-purity gold raw material is 1 kg-3 kg; the shape of the high-purity gold raw material comprises granular shape, powdery shape and flaky shape.
4. The method for manufacturing the fixed-point furnace gold fixed-point bottle according to claim 3, wherein the high-purity gold raw material is granular high-purity gold with the diameter of 3-5 mm.
5. The method for manufacturing the fixed-point furnace fixed-point bottle according to claim 1, wherein in the step 2, the quartz bottle is vacuumized to a vacuum degree of less than 1 Pa; filling high-purity argon with 1 standard atmosphere, wherein the purity of the argon is more than or equal to 99.99 percent.
6. The method for manufacturing the fixed-point furnace fixed-point bottle according to claim 5, wherein in the step 2, the quartz bottle is vacuumized until the vacuum degree is less than or equal to 0.1 Pa.
7. The method for manufacturing the fixed-point furnace gold fixed-point bottle according to claim 1, wherein in the step 6, the specific operation steps comprise:
step 61, measuring the temperature related information of the high-purity gold in the quartz bottle by adopting a thermocouple; setting the temperature of the fixed point furnace to 1060 ℃, and starting to measure the potential value of the thermocouple;
step 62, setting the temperature of the fixed-point furnace to be 1080 ℃, melting the high-purity gold in the quartz bottle, and obtaining a melting temperature plateau of the high-purity gold according to the measured value;
and step 63, setting the temperature of the fixed-point furnace to 1060 ℃, starting to reduce the temperature, and obtaining the solidification temperature plateau of the high-purity gold according to the measured value.
8. The method for manufacturing the fixed point furnace gold fixed point bottle according to claim 7, wherein three standard S or R type thermocouples which are distributed in a step shape with equal height are inserted into the quartz bottle, and the related information of the temperature of the high-purity gold in the quartz bottle is measured.
9. The method for manufacturing a fixed-point furnace gold fixed-point bottle according to claim 1, wherein the vacuumizing and inflating operations described in step 2 are performed by using a sealed protective sleeve; the sealing protective sleeve comprises a lower assembly main body (1) and an upper assembly main body (5) which are mutually detachable, hermetically matched and the lower assembly main body (1) and the upper assembly main body (5) are both in an annular structure and are sequentially sealed and arranged at the upper port of the fixed point bottle from bottom to top in a sealing manner; go up and be equipped with air exhaust pipeline (10) and gas pipeline (11) on subassembly main part (5), air exhaust pipeline (10) are used for communicateing fixed point bottle internal environment and outside air exhaust equipment, gas pipeline is used for communicateing fixed point bottle and outside gas equipment.
10. The manufacturing method of the fixed point furnace gold fixed point bottle according to claim 9, characterized in that a plurality of lower assembly bolt holes (4) are arranged on the lower assembly main body (1), and the plurality of lower assembly bolt holes (4) are uniformly distributed along the circumferential direction of the lower assembly main body (1); a plurality of upper assembly bolt holes (8) are formed in the upper assembly main body (5), and the plurality of upper assembly bolt holes (8) are uniformly distributed along the annular direction of the upper assembly main body (5); the upper assembly main body (5) and the lower assembly main body (1) are detachably connected through the bolt sequentially penetrating the upper assembly bolt hole (8) and the corresponding lower assembly bolt hole (4).
11. The method for manufacturing a fixed-point furnace gold fixed-point bottle according to claim 9, wherein the lower assembly body (1) further comprises a lower assembly O-shaped sealing ring (2), and the upper assembly body (5) further comprises an upper assembly O-shaped sealing ring (6); lower subassembly O type sealing washer (2) and last subassembly O type sealing washer (6) all overlap and establish fixed point bottle port outer wall department, lower subassembly O type sealing washer (2) and last subassembly O type sealing washer (6) compress tightly to be fixed between last subassembly main part (5) and lower subassembly main part (1), and all with fixed point bottle outer wall sealing contact.
12. The manufacturing method of the fixed point gold furnace fixing point bottle as claimed in claim 9, wherein a sealing cover (9) is arranged on the upper assembly body (5), and the sealing cover (9) is hermetically covered on the top port of the annular structure of the upper assembly body (5); the sealing cover (9) is provided with a through hole for communicating the air exhaust pipeline (10) and the air inflation pipeline (11) with the fixed point bottle.
13. The method for manufacturing the fixed point gold bottle of the fixed point furnace according to any one of claims 9 to 12, wherein the lower module body (1) is internally provided with a lower module cooling chamber which is continuously distributed along a ring direction, and a coolant is introduced into the lower module cooling chamber through a lower module cooling pipeline (3); an upper assembly cooling cavity which is continuously distributed along the annular direction is arranged in the upper assembly main body (5), and a coolant is introduced into the lower assembly cooling cavity through an upper assembly cooling pipeline (7).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911234075.5A CN111044179B (en) | 2019-12-05 | 2019-12-05 | Method for manufacturing fixed point furnace gold fixed point bottle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911234075.5A CN111044179B (en) | 2019-12-05 | 2019-12-05 | Method for manufacturing fixed point furnace gold fixed point bottle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111044179A CN111044179A (en) | 2020-04-21 |
| CN111044179B true CN111044179B (en) | 2022-01-04 |
Family
ID=70234684
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911234075.5A Active CN111044179B (en) | 2019-12-05 | 2019-12-05 | Method for manufacturing fixed point furnace gold fixed point bottle |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111044179B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08114507A (en) * | 1994-10-17 | 1996-05-07 | Tanaka Kikinzoku Kogyo Kk | Calibrating method for fixed point of thermocouple |
| US6398405B1 (en) * | 1998-12-11 | 2002-06-04 | Agency Of Industrial Science And Technology | Fixed-point crucible, fixed-point temperature realizing apparatus using the crucible and temperature calibration method |
| CN206557138U (en) * | 2016-12-29 | 2017-10-13 | 中南大学 | A kind of device tested the behavior of metal material rapid solidification and solidify hot-fluid |
| CN109323768A (en) * | 2018-10-19 | 2019-02-12 | 中国计量科学研究院 | A kind of self calibration blackbody radiation source |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3436006B2 (en) * | 1996-07-29 | 2003-08-11 | 日亜化学工業株式会社 | Reducing atmosphere furnace with hydrogen gas circulation |
| JP4639383B2 (en) * | 2006-02-24 | 2011-02-23 | 独立行政法人産業技術総合研究所 | Temperature fixed point cell, temperature fixed point device, and thermometer calibration method |
| CN201600202U (en) * | 2009-09-11 | 2010-10-06 | 中国计量科学研究院 | Sealing type zinc and tin freezing point container |
| CN201867055U (en) * | 2010-11-09 | 2011-06-15 | 上海嘉翎电子科技有限公司 | Tungsten-rhenium thermocouple fuse fixed-point furnace |
| CN202677219U (en) * | 2012-06-14 | 2013-01-16 | 西安航天计量测试研究所 | Low-temperature continuous point temperature control thermostat |
| CN108344764A (en) * | 2018-03-13 | 2018-07-31 | 华侨大学 | Low-temperature high-vacuum composite heating platform |
-
2019
- 2019-12-05 CN CN201911234075.5A patent/CN111044179B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08114507A (en) * | 1994-10-17 | 1996-05-07 | Tanaka Kikinzoku Kogyo Kk | Calibrating method for fixed point of thermocouple |
| US6398405B1 (en) * | 1998-12-11 | 2002-06-04 | Agency Of Industrial Science And Technology | Fixed-point crucible, fixed-point temperature realizing apparatus using the crucible and temperature calibration method |
| CN206557138U (en) * | 2016-12-29 | 2017-10-13 | 中南大学 | A kind of device tested the behavior of metal material rapid solidification and solidify hot-fluid |
| CN109323768A (en) * | 2018-10-19 | 2019-02-12 | 中国计量科学研究院 | A kind of self calibration blackbody radiation source |
Non-Patent Citations (1)
| Title |
|---|
| 基于准绝热的锌固定点复现装置;王伟等;《计量学报》;20161122(第06期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111044179A (en) | 2020-04-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20080175936A1 (en) | Nano-Precision Sintering System | |
| CN111044179B (en) | Method for manufacturing fixed point furnace gold fixed point bottle | |
| CN103162537A (en) | Device and method for sintering sinter products | |
| CN109990906B (en) | High-temperature high-pressure closed cavity infrared temperature measurement system and method | |
| CN108754198A (en) | A kind of preparation method of flexibility block metal glass | |
| KR101031079B1 (en) | Apparatus for measuring level of blast furnace bucket material | |
| CN205958129U (en) | Retractable thermocouple thermometer | |
| Nikolaev et al. | Purification of Alkali-Metal Chlorides by Zone Recrystallization for Use in Pyrochemical Processing of Spent Nuclear Fuel | |
| CN204768764U (en) | Hyperbar environmental test case | |
| CN210981590U (en) | Protective sleeve for preparing fixed-point bottle | |
| CN111063458B (en) | Device and method for accurately calibrating plasma injection impurities | |
| Lowe et al. | Reproducible metal–carbon eutectic fixed-points | |
| CN100569985C (en) | A kind of Zirconium based amorphous alloy | |
| CN107829049B (en) | Titanium-containing zirconium-based block amorphous alloy and preparation process thereof | |
| CN106226345B (en) | Quasi-adiabatic minitype gallium phase change fixed point device and measuring method | |
| CN210166034U (en) | High-temperature high-pressure closed intracavity infrared temperature measurement system | |
| CN208546525U (en) | A kind of vacuum screened sealing structure and the equipment for being equipped with vacuum screened sealing structure | |
| CN217468000U (en) | High-temperature test equipment for LOCA working condition cladding material | |
| JP5754636B2 (en) | Germanium melt molding method and apparatus | |
| CN113275543B (en) | Counter-gravity filling cabin for large-size complex amorphous alloy component | |
| CN216838277U (en) | Device for producing ultra-high-purity arsenic rod | |
| CN107964639B (en) | Carbon and iron-containing zirconium-based block amorphous alloy and preparation process thereof | |
| JP2013154373A (en) | Method of melt molding germanium | |
| CN104971786A (en) | High atmospheric pressure environmental test chamber | |
| CN116698199B (en) | Radial heat flow sensor based on atomic layer thermopile and installation test method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |