CN103602906B - Heating element for synthesizing diamond - Google Patents

Heating element for synthesizing diamond Download PDF

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CN103602906B
CN103602906B CN201310576164.4A CN201310576164A CN103602906B CN 103602906 B CN103602906 B CN 103602906B CN 201310576164 A CN201310576164 A CN 201310576164A CN 103602906 B CN103602906 B CN 103602906B
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metal
heater
heating tube
cold wind
heating
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CN103602906A (en
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蔡立超
范建朝
冷树良
姬鹏鹤
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Shandong Liaocheng Laixin Superhard Material Co Ltd
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Shandong Liaocheng Laixin Superhard Material Co Ltd
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Abstract

The invention relates to a heating element for synthesizing diamond. The heating element is characterized by comprising heating tubes and heating sheets, wherein the heating tubes are made from alloy, and the alloy is prepared from the following raw materials in percentage by mass: 10-22% of purified chromium metal, 3-8% of molybdenum metal, 2-5% of titanium metal and the balance of ferrous metal. According to the heating element disclosed by the invention, the resistance is 1.9-2.6 micro-ohm.m (at the temperature of 20 DEG C), so that the electric energy utilization ratio is high; the wall thickness is thin and can reach 0.02mm to the thinnest, so that the volume of a synthesis cavity can be increased, and the yield is increased; the wall thickness of the heating element disclosed by the invention can be thinner, and shown by test detection, under the condition that the wall thickness is 0.04mm, the resistance value is highest and the electric energy utilization ratio is optimal.

Description

Diamond synthesis heating unit
Technical field
The present invention relates to a kind of diamond synthesizing heating member, is exactly a kind of diamond synthesis heating unit.
Background technology
Man-made diamond synthesizes at high temperature under high pressure, and synthesis device is six-plane piercer mainly.The required high temperature of synthesis adopts the mode indirect heating to the heating unit electrified regulation in Synthetic block.The Synthetic block of current indirect heating manner lives outer race steel bowl for synthesizing core, and steel bowl periphery is coated with insulating layer coating, insulation layer outer race heating unit.Current existing heating unit is heating tube and heating piece, and material is graphite sheet.The resistance of this heating unit is lower, and wall thickness is thicker, and therefore utilization rate of electrical is low, and synthetic cavity is little, impact synthesis output.
Summary of the invention
For solving the problem, the object of this invention is to provide a kind of diamond synthesis heating unit.
Diamond synthesis heating unit, comprises heating tube and heating piece, and heating piece spiral-lock is on heating tube, the material of heating tube is alloy, and alloy is made up of the raw material of following mass percent: the chromium metal 10-22% of purifying, molybdenum 3-8%, titanium metal 2-5%, surplus is ferrous metal.
The material of described heating piece is graphite sheet.
The thickness of described heating tube is 0.02-0.05mm.
The making method of described heating tube is: 1. inserted by chromium metal in 80 DEG C of potassium bromate solution, ultrasonic vibration 1 minute, then use distilled water flushing 2 minutes, dries, obtains the chromium metal of purifying; 2. get raw material by following weight percent: the chromium metal 10-22% of purifying, molybdenum 3-8%, titanium metal 2-5%, surplus is ferrous metal; 3. the chromium metal of molybdenum, titanium metal, ferrous metal and purifying being added melting in smelting furnace, obtain blank, is alloyed metal band by blank forging and stamping; 4. just 3. step prepares the shearing of alloyed metal band, and the length of the metal strip after shearing is identical with the girth preparing shaping heating tube; Metal cleaner alloy metallic strip surface is used to clean; Alloyed metal tape welding is connected into tubulose; 5. the metal strip of tubulose carries out hydrogen atmosphere and sinters 1 hour inserting in sintered quenching integrated furnace, then carries out air blast quenching process, obtains heating tube.
The heating tube that 5. step is prepared inserts concentrated nitric acid 20s, wiped clean after taking out.
In the preparation method of described heating tube step 5. in sintered quenching integrated furnace comprise body of heater, bottom of furnace body arranges hydrogen gas pipe 4, evenly arranges severally to connect heat pipe in body of heater; Several fixed ring is set in body of heater, fixed ring hierarchal arrangement, the side of fixed ring is connected by fixed handle with inboard wall of furnace body, fixed ring is uniformly distributed several permanent seat, permanent seat is roundedly uniformly distributed montant and annulus forms by several, annulus will be connected with each montant, and fixed ring arranges permanent seat place and offers through hole; Body of heater is installed whipping appts and breather, whipping appts and breather coordinate with body of heater respectively, described whipping appts is made up of capping, agitator motor, stir shaft, paddle, capping coordinates with the top of body of heater, capping top arranges agitator motor, and capping bottom arranges stir shaft, and stir shaft is connected with the output shaft of agitator motor, stir shaft arranges paddle, and stir shaft is through fixed ring; Described breather is connected and composed by top cover, cold wind inlet pipe 4, ring pipe, several cold wind arm, top cover coordinates with the top of body of heater, ring pipe is installed on top cover top, ring pipe connects cold wind inlet pipe 4, ring pipe bottom arranges cold wind arm, and cold wind arm sets out air port, is penetrating hole bottom cold wind arm, cold wind arm is through through hole, and the height of air outlet is identical with permanent seat position.Described bottom of furnace body is arcuate bottom.
The invention has the advantages that: heater element resistance of the present invention is 1.9-2.6u Ω m(20 DEG C), therefore utilization rate of electrical is high; Wall thickness is thin, the thinlyyest can reach 0.02mm, can increase the volume of synthetic cavity, increase yield; The wall thickness of heating unit of the present invention can be thinner, and after testing, wall thickness is that under 0.04mm condition, resistance value is the highest, and utilization rate of electrical is best.Heating tube bulk strength is high, thermal conductivity good, and compared with the heating tube of other alloys, treated chromium metal strip no longer includes the impurity of the chromium sesquioxide of oxidation, and in alloy, impurity is few, purity is high, good heat conduction effect; Have solution strengthening effect between titanium and molybdenum, moulding height under low-temperature condition, is convenient to shape; Molybdenum can increase thermal conductivity and the low coefficient of expansion, and at high temperature (1100 ~ 1650 DEG C) have high intensity.
Accompanying drawing explanation
Fig. 1 is one of structural representation of the present invention; Fig. 2 is the sectional structure schematic diagram along Figure 1A-A line; Fig. 3 is structural representation two of the present invention; Fig. 4 is the structural representation of whipping appts of the present invention; Fig. 5 is breather structural representation of the present invention; Fig. 6 is the plan structure schematic diagram of Fig. 5; Fig. 7 is the I partial enlargement structural representation of Fig. 1.
Reference numeral: 1 agitator motor 2 capping 3 stir shaft 4 hydrogen gas pipe 5 fixed handle 6 fixed ring 7 permanent seat 8 metal strip 9 paddle 10 body of heater 11 heating tube 12 arcuate bottom 13 through hole 14 cold wind inlet pipe 15 ring pipe 16 top cover 17 cold wind arm 18 air outlet.
Embodiment
Diamond synthesis heating unit, comprises heating tube and heating piece, and heating piece spiral-lock is on heating tube, the material of heating tube is alloy, and alloy is made up of the raw material of following mass percent: the chromium metal 10-22% of purifying, molybdenum 3-8%, titanium metal 2-5%, surplus is ferrous metal.
Prepare every 1000g alloy to be made up of following raw material:
1, the chromium metal 100g of purifying, molybdenum 30g, titanium metal 20g, ferrous metal 850g: resistance is 1.9u Ω m(20 DEG C), wall thickness 0.05mm; 2, the chromium metal 160g of purifying, molybdenum 50g, titanium metal 40g, ferrous metal 750g: resistance is 2.3u Ω m(20 DEG C), wall thickness 0.02mm; 3, the chromium metal 220g of purifying, molybdenum 80g, titanium metal 50g, ferrous metal 650g: resistance is 2.2u Ω m(20 DEG C), wall thickness 0.03mm;
4, the chromium metal 180g of purifying, molybdenum 70g, titanium metal 30g, ferrous metal 720g: resistance is 2.6u Ω m(20 DEG C), wall thickness 0.04mm.
The material of described heating piece is graphite sheet, and heating piece can adopt alloy, can improve utilization rate of electrical further.But preferably adopt graphite sheet, due to heating piece and diamond contact limited area, the utilization rate of electrical of raising is limited, so still adopt graphite sheet, reduce production cost.
The making method of described heating tube is: 1. inserted by chromium metal in 80 DEG C of potassium bromate solution, ultrasonic vibration 1 minute, then use distilled water flushing 2 minutes, dries, obtains the chromium metal of purifying; Chromium metallic surface is oxidized formation chromium sesquioxide in atmosphere, after this step process, chromium sesquioxide is dissolved in potassium bromate solution, avoid in heating tube containing chromium sesquioxide, affect the quality of heating tube, put forward heavy alloyed purity, avoid, because impurity produces the intensity of further Oxidative demage heating tube, increasing the life-span of heating tube; Ultrasonic vibration can accelerate the dissolution rate of chromium sesquioxide, reduces the time of this step, increases efficiency; Distilled water flushing keeps chromium metallic surface to clean, and removes the potassium bromate remaining in surface.2. get raw material by following weight percent: the chromium metal 10-22% of purifying, molybdenum 3-8%, titanium metal 2-5%, surplus is ferrous metal; The chromium metal of the purifying 3. molybdenum, titanium metal, ferrous metal and step 2. prepared adds melting in smelting furnace, obtains blank, is alloyed metal band by blank forging and stamping.After melting and forging and stamping, each metal effectively disperses, and keeps stability and the consistence at each position of alloyed metal band.4. just 3. step prepares the shearing of alloyed metal band, and the length of the metal strip after shearing is identical with the girth preparing shaping heating tube; Metal cleaner alloy metallic strip surface is used to clean; By the Impurity removal of alloyed metal belt surface after cleaning, avoid the quality that the impurity effect of next step welding process interalloy metallic strip surface welds, improve welding quality; Alloyed metal tape welding is connected into tubulose; 5. the metal strip of tubulose carries out hydrogen atmosphere and sinters 1 hour inserting in sintered quenching integrated furnace, then carries out air blast quenching process, obtains heating tube.Sinter in hydrogen atmosphere, residual oxide compound can be reduced, improve the purity of heating tube, improve resistance; Air blast quenching can carry out a modification by alloy, further resistance value is improved 10%, increases utilization rate of electrical.The heating tube that 5. step is prepared inserts concentrated nitric acid 20s, wiped clean after taking out.Metal tube surface is rapid passivation in concentrated nitric acid, and surface produces layer protecting film, avoids metal tube long-term oxidized in atmosphere, improves the life-span of metal tube.
The metal strip of tubulose can sinter in common hydrogen atmosphere sintering oven, be transferred to again in air blast quenching stove and carry out quench treatment, but due to the singularity of its structure, do not have a kind of hydrogen atmosphere sintering oven and air blast quenching stove to meet above-mentioned requirements at present.And in transfer process, easily damage the tubular metal band under the condition of high temperature, cause damage.In order to overcome the problems referred to above, as shown in figures 1 and 3, described sintered quenching integrated furnace comprises body of heater 10, hydrogen gas pipe 4 is set bottom body of heater 10, hydrogen enters body of heater 10 by bottom, because air is gently upwards extruded by hydrogen quality, logical hydrogen can be stopped when hydrogen atmosphere is tested at body of heater 10 top.Evenly arrange in body of heater 10 and severally connect heat pipe 11, heating tube 11 improves temperature for body of heater 10, and several heating tube 11 is uniformly distributed, and the temperature at each position in body of heater 10 is improved simultaneously.As shown in Figure 2, several fixed ring 6 is set in body of heater 10, fixed ring 6 hierarchal arrangement, effectively utilizes the space of body of heater 10, and the side of fixed ring 6 is connected by fixed handle 5 with body of heater 10 inwall, fixed ring 6 is uniformly distributed several permanent seat 7, metal strip 8 is sleeved on permanent seat 7, and as shown in Figure 7, permanent seat 7 is roundedly uniformly distributed montant and annulus forms by several, annulus will be connected with each montant, and when this structure facilitates air blast quenching, cold wind passes through.Fixed ring 6 arranges permanent seat 7 place and offers through hole 13.Body of heater 10 is installed whipping appts and breather, whipping appts and breather coordinate with body of heater 10 respectively.Adopt whipping appts in hydrogen atmosphere sintering process, air blast quenching process adopts breather.As shown in Figure 4, described whipping appts is made up of capping 2, agitator motor 1, stir shaft 3, paddle 9, capping 2 coordinates with the top of body of heater 10, capping 2 top arranges agitator motor 1, capping 2 bottom arranges stir shaft 3, stir shaft 3 is connected with the output shaft of agitator motor 1, stir shaft 3 is arranged paddle 9, stir shaft 3 is through fixed ring 6, the hydrogen atmosphere of heating fully mixes by whipping appts in hydrogen atmosphere sintering process, keep each spot temperature even, paddle 9, at different heights, can keep the temperature equilibrium of every aspect.As shown in Figure 5 and Figure 6, described breather is connected and composed by top cover 16, cold wind inlet pipe 14, ring pipe 15, several cold wind arm 17, top cover 16 coordinates with the top of body of heater 10, ring pipe 15 is installed on top cover 16 top, and ring pipe 15 connects cold wind inlet pipe 14, ring pipe 15 bottom arranges cold wind arm 17, cold wind arm 17 sets out air port 18, be penetrating hole bottom cold wind arm 17, cold wind arm 17 is through through hole 13, and the height of air outlet 18 is identical with permanent seat 7 position.Taken off by whipping appts after having sintered, be arranged on by breather on body of heater 10, enter cold wind by cold wind inlet pipe 14, cold wind is dispensed to each cold wind arm 17 by ring pipe 15, is ejected on metal strip 8 inwall by the air outlet on cold wind arm 17.Be arcuate bottom 12 bottom described body of heater 10, cold wind is discharged bottom cold wind arm 17 again simultaneously, produces internal recycling, be upwards ejected on the outer wall of metal strip 8 through arcuate bottom 12.Hydrogen atmosphere sintering and cold wind quenching can realize by this device in the same apparatus, avoid damaging in metal strip transfer process, improve the quality of metal strip.Metal strip coordinates completely with this device, and fully, cold wind uniform quenching, ensures carrying out efficiently of this step to hydrogen atmosphere sintering.
The working process of described sintered quenching integrated furnace is: be sleeved on permanent seat 7 by metal strip 8, then in body of heater 10, passes into hydrogen by hydrogen gas pipe 4, when body of heater 10 top hydrogen detected time, stop ventilation.Whipping appts is arranged on body of heater 10, is sealed by capping 2, start agitator motor 1 and stir, carry out heat-agglomerating by heating tube 11 simultaneously.After having sintered, take off whipping appts, be arranged on by breather on body of heater 10, the cold wind inlet pipe 14 to notifying device leads to cold wind, carries out air blast quenching.
Technical scheme of the present invention is not restricted in the scope of embodiment of the present invention.The technology contents of the not detailed description of the present invention is known technology.

Claims (6)

1. diamond synthesis heating unit, it is characterized in that: comprise heating tube and heating piece, heating piece spiral-lock is on heating tube, the material of heating tube is alloy, alloy is made up of the raw material of following mass percent: the chromium metal 10-22% of purifying, molybdenum 3-8%, titanium metal 2-5%, surplus is ferrous metal;
The making method of described heating tube is:
1. chromium metal is inserted in 80 DEG C of potassium bromate solution, ultrasonic vibration 1 minute, then use distilled water flushing 2 minutes, dry, obtain the chromium metal of purifying;
2. get raw material by following weight percent: the chromium metal 10-22% of purifying, molybdenum 3-8%, titanium metal 2-5%, surplus is ferrous metal;
3. the chromium metal of molybdenum, titanium metal, ferrous metal and purifying being added melting in smelting furnace, obtain blank, is alloyed metal band by blank forging and stamping;
4. 3. step is prepared alloyed metal band to shear, the length of the metal strip after shearing is identical with the girth preparing shaping heating tube; Metal cleaner alloy metallic strip surface is used to clean; Alloyed metal tape welding is connected into tubulose;
5. the metal strip of tubulose carries out hydrogen atmosphere and sinters 1 hour inserting in sintered quenching integrated furnace, then carries out air blast quenching process, obtains heating tube.
2. according to diamond synthesis heating unit according to claim 1, it is characterized in that: the material of described heating piece is graphite sheet.
3. diamond synthesis heating unit according to claim 1, is characterized in that: the thickness of described heating tube is 0.02-0.05mm.
4. diamond synthesis heating unit according to claim 1, is characterized in that: the heating tube that 5. step is prepared inserts concentrated nitric acid 20s, wiped clean after taking out.
5. diamond synthesis heating unit according to claim 1, it is characterized in that: in the preparation method of described heating tube step 5. in sintered quenching integrated furnace comprise body of heater (10), body of heater (10) bottom arranges hydrogen gas pipe (4), evenly arranges and severally connect heat pipe (11) in body of heater (10), several fixed ring (6) is set in body of heater (10), fixed ring (6) hierarchal arrangement, the side of fixed ring (6) is connected by fixed handle (5) with body of heater (10) inwall, fixed ring (6) is uniformly distributed several permanent seat (7), permanent seat (7) is roundedly uniformly distributed montant and annulus forms by several, annulus will be connected with each montant, and fixed ring (6) arranges permanent seat (7) place and offers through hole (13), body of heater (10) is upper installs whipping appts and breather, whipping appts and breather coordinate with body of heater (10) respectively, described whipping appts is made up of capping (2), agitator motor (1), stir shaft (3), paddle (9), capping (2) coordinates with the top of body of heater (10), capping (2) top arranges agitator motor (1), capping (2) bottom arranges stir shaft (3), stir shaft (3) is connected with the output shaft of agitator motor (1), stir shaft (3) is arranged paddle (9), stir shaft (3) is through fixed ring (6), described breather is by top cover (16), cold wind inlet pipe (14), ring pipe (15), several cold wind arm (17) connects and composes, top cover (16) coordinates with the top of body of heater (10), ring pipe (15) is installed on top cover (16) top, ring pipe (15) is upper connects cold wind inlet pipe (14), ring pipe (15) bottom arranges cold wind arm (17), cold wind arm (17) sets out air port (18), cold wind arm (17) bottom is penetrating hole, cold wind arm (17) is through through hole (13), the height of air outlet (18) is identical with permanent seat (7) position.
6. diamond synthesis heating unit according to claim 5, is characterized in that: described body of heater (10) bottom is arcuate bottom (12).
CN201310576164.4A 2013-11-18 2013-11-18 Heating element for synthesizing diamond Active CN103602906B (en)

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Publication number Priority date Publication date Assignee Title
CN107091574A (en) * 2016-05-16 2017-08-25 湖南天源工业设备有限公司 A kind of atmosphere sintering furnace
CN113290926B (en) * 2021-04-26 2021-11-05 杭州超然金刚石有限公司 Preparation device and preparation process of diamond semiconductor

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SE439497B (en) * 1977-02-15 1985-06-17 Centre Rech Metallurgique USING AN ALLOY
CN2889475Y (en) * 2006-01-24 2007-04-18 蔡博 Indirect heating synthetic block assembly for diamond synthesis
CN101279223B (en) * 2008-05-05 2010-11-17 江苏工业学院 Use of electrothermal alloy in six-side top high-temperature high-pressure synthetic cavity
CN201906593U (en) * 2010-12-29 2011-07-27 山东聊城昌润超硬材料有限公司 Indirect heating device for diamond synthesis

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