CN111922350B - Preparation method of low-hydrochloric-acid-insoluble metal chromium powder - Google Patents
Preparation method of low-hydrochloric-acid-insoluble metal chromium powder Download PDFInfo
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 19
- 239000002184 metal Substances 0.000 title claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N hydrochloric acid Substances Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 83
- 238000005245 sintering Methods 0.000 claims abstract description 67
- 239000011812 mixed powder Substances 0.000 claims abstract description 54
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 49
- 239000011651 chromium Substances 0.000 claims abstract description 49
- 239000000843 powder Substances 0.000 claims abstract description 39
- 238000000227 grinding Methods 0.000 claims abstract description 20
- 238000011049 filling Methods 0.000 claims abstract description 14
- 238000003825 pressing Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000000748 compression moulding Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000006392 deoxygenation reaction Methods 0.000 claims description 14
- 238000004321 preservation Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 5
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 5
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 5
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 238000010408 sweeping Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 9
- 238000004663 powder metallurgy Methods 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 229960000443 hydrochloric acid Drugs 0.000 description 38
- 238000002474 experimental method Methods 0.000 description 16
- 238000002844 melting Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
Abstract
The invention discloses a preparation method of low-hydrochloric acid insoluble metal chromium powder, which comprises the following steps: s1 preparation of chromium powder: grinding and crushing the chromium blocks at low temperature to prepare powder, and controlling the temperature to be-150-0 ℃ to obtain chromium powder; s2 powder mixing: adding a deoxidizing agent into the prepared chromium powder, wherein the addition proportion is 0.1-5 wt%, and keeping the materials uniformly mixed to obtain mixed powder; s3 pressing: filling the mixed powder into a mold, and pressing the mixed powder into a blank block by compression molding, wherein the pressure parameter is 5-20 MPa; s4 sintering: putting the pressed chromium blank into a vacuum sintering furnace for sintering; s5 powder preparation: and grinding and crushing the sintered chromium blank at a low temperature to prepare powder, and controlling the temperature to be-150-0 ℃ to obtain the low-hydrochloric-acid-insoluble metal chromium powder. Compared with chromium powder prepared by the traditional process, the content of hydrochloric acid insoluble substances of the chromium powder prepared by the invention is obviously reduced, the use effect of chromium powder metallurgy products is obviously improved, and the service life of the chromium powder metallurgy products is obviously prolonged.
Description
Technical Field
The invention relates to the technical field of metal powder preparation, in particular to a preparation method of low-hydrochloric-acid-insoluble metal chromium powder.
Background
The term "hydrochloric acid-insoluble substance" generally means a substance insoluble in dilute hydrochloric acid (10% to 20% hydrochloric acid). In the chromium powder, the insoluble matter is Al2O3、Fe2O3And SiO2For example, the content of acid-insoluble substances is low, and this is one of the indexes for inspecting the quality of powder.
Hazard of acid insoluble substance: the inclusion formed by the acid-insoluble substances in the sintered part of the powder metallurgy part is easy to become a crack source when stressed, the strength of the sintered part is damaged, and particularly, when the sintered part bears fatigue load, cracks are likely to be generated at the inclusion part, so that the part fails, and the fatigue life of the part is reduced.
Therefore, a preparation method is needed for reducing and controlling the content of the insoluble hydrochloric acid in the chromium powder, so that the problems caused by applying the chromium powder to a powder metallurgy product and influencing the production and use are avoided.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of low-hydrochloric-acid-insoluble metal chromium powder.
The technical scheme of the invention is as follows: a preparation method of low-hydrochloric-acid-insoluble metal chromium powder comprises the following steps:
s1 preparation of chromium powder: grinding and crushing the chromium blocks at low temperature to prepare powder, and controlling the temperature to be-150-0 ℃ to obtain chromium powder;
s2 powder mixing: adding a deoxidizer into the chromium powder obtained in the step S1, wherein the addition proportion is 0.1-5 wt%, and uniformly mixing the materials to obtain mixed powder;
s3 pressing: filling the mixed powder obtained in the step S2 into a mold, and pressing the mixed powder into a blank block by compression molding to obtain a chromium blank, wherein the pressure parameter is 5-20 MPa;
s4 sintering: putting the chromium blank obtained in the step S3 into a vacuum sintering furnace for sintering to obtain a sintered chromium blank;
s5 powder preparation: and (5) carrying out low-temperature grinding and crushing on the sintered chromium blank in the step (S4) to prepare powder, and controlling the temperature to be-150-0 ℃ to obtain the low-hydrochloric-acid-insoluble metal chromium powder.
Further, the deoxidizer is graphite powder. The deoxidizing agent adopts graphite powder, has low cost and good economy, has excellent deoxidizing effect when being used for preparing the chromium powder with low hydrochloric acid insoluble substances, and can ensure that the prepared chromium powder has lower hydrochloric acid insoluble substances.
Further, in the step S4, the sintering temperature is controlled to be 1000-1500 ℃, the heat preservation time is 30-480 min, and the vacuum degree is less than 100 Pa. By the parameters such as the sintering temperature and the like, the prepared chromium block has compact crystalline phase and low oxygen content, and the percentage content of hydrochloric acid insoluble substances thereof is low.
Further, the sintering in step S4 is specifically:
1) putting the chromium blank obtained in the step S3 into a vacuum sintering furnace with the vacuum degree less than 100 Pa, heating to 450-550 ℃ at the speed of 5 ℃/min, and keeping the temperature for 10-30 min;
2) heating to 800-900 ℃ from 450-550 ℃ at a speed of 10 ℃/min, and keeping the temperature for 10-30 min;
3) raising the temperature from 800-900 ℃ at a speed of 5 ℃/min to 1000-1500 ℃, and keeping the temperature for 30-480 min.
Through the gradient temperature rising sintering, the graphite powder and the chromium powder have different temperature rising rates at the front section, the middle section and the rear section of the sintering, so that more sufficient conditions are provided for the mixed reaction of the graphite powder and the chromium powder in the mixed powder, the deoxidation effect of the graphite powder deoxidizer is improved, and the chromium powder with lower hydrochloric acid insoluble substances is obtained.
Further, in the steps S1 and S5, liquid nitrogen is introduced into the powder for grinding at low temperature to prepare powder, and the liquid nitrogen is used as a protective medium. By carrying out low-temperature crushing and grinding under the protection of liquid nitrogen, powder with a finer particle size can be obtained, and the low-temperature crushing and grinding can ensure that the tissue components of the crushed substances are not damaged.
Further, before the pressing in step S3, the mixed powder is filled into the mold in a layered filling manner, which specifically includes the following steps:
1) uniformly spraying the mixed powder obtained in the step S2 into a die through a powder sprayer, and continuously accumulating the thickness of the mixed powder to form a mixed powder layer, wherein the thickness of the mixed powder layer is 1-2 mm, and the uniformly spraying dosage on the mixed powder layer is 5-10 ml/cm2The deoxygenation liquid of (1);
2) then, a pulse laser emits a laser beam, the laser beam is focused into a laser line or a laser band through a laser focusing system, the mixed powder layer is rapidly irradiated from left to right through scanning of the laser line or the laser band to be slightly melted, and the surface density of the mixed powder layer is controlled to be 50-70%, wherein the laser energy density is 6-9 mJ/mm2The distance between the laser line or the laser band and the surface of the mixed powder layer is 35-45 mm, and the sweeping speed of the laser line or the laser band is 1-2 cm/s;
3) after laser beam scanning, the surface is quickly and uniformly sprayed with 5-10 ml/cm of spray dosage2Reducing the surface temperature of the deoxidizing liquid to 10-15 ℃;
4) and (3) repeating the steps 1) and 3) for multiple times until the mixed powder is completely filled into a mold, and then performing compression molding to obtain a compact, thereby obtaining the chromium blank.
Through the layered filling mode, the mixed powder layer can be in full contact with graphite powder and the like in the deoxygenation liquid, the mixed powder layer is slightly melted by laser sweep with the power, the deoxygenation effect of the chromium powder by the graphite powder is improved, and the chromium powder with lower content of hydrochloric acid insoluble substances is obtained by matching with the subsequent sintering steps and the like.
Furthermore, the deoxygenation liquid in the step 1) and the step 3) comprises, by weight, 10-15 parts of graphite powder, 2-3 parts of polyethylene glycol, 1-2 parts of hydroxypropyl methyl cellulose and 20-30 parts of ethanol; wherein the particle size of the graphite powder is 0.02-0.05 mm;
the preparation method of the deoxygenation liquid comprises the following steps: adding graphite powder into water, continuously stirring, sequentially dropwise adding polyethylene glycol and hydroxypropyl methyl cellulose, and continuously stirring to obtain a suspension, wherein the deoxygenation liquid needs to be prepared for use on site and needs to be uniformly stirred before use.
The prepared deoxidizing liquid can further improve the deoxidizing effect on the chromium powder, and effectively cooperates with laser scanning slight melting to carry out micro-melting layered integration on the chromium powder, so that the subsequent sintering effect is improved, and the content of the hydrochloric acid insoluble substances of the prepared chromium powder is reduced.
Further, the cooling treatment after sintering in step S4 is specifically: and closing the vacuum sintering furnace, and naturally cooling the sintered chromium blank in the furnace to room temperature in an argon atmosphere.
The invention has the beneficial effects that:
(1) the preparation method prepares the chromium blocks by mixing the chromium powder and the deoxidizer graphite powder and prepares the chromium blocks into powder, and the content of the hydrochloric acid insoluble substance of the prepared chromium powder is obviously reduced compared with the chromium powder prepared by the traditional process, so that the method can effectively prevent the sintered parts of the chromium powder metallurgy parts from easily generating cracks when stressed, and influencing the use effect and the service life of the parts.
(2) According to the preparation method, the mixed powder layer can be fully contacted with the graphite powder and the like in the deoxygenation liquid in a layered filling mode, the mixed powder layer is slightly melted through laser scanning, the deoxygenation effect of the chromium powder by the graphite powder is improved, and the chromium powder with lower content of hydrochloric acid insoluble substances is obtained by matching with the subsequent sintering and other steps.
Drawings
FIG. 1 is a process flow diagram of the preparation method of the present invention.
Detailed Description
Example 1
A preparation method of low-hydrochloric-acid-insoluble metal chromium powder comprises the following steps:
s1 preparation of chromium powder: grinding and crushing the chromium blocks at low temperature to prepare powder, introducing liquid nitrogen as a protective medium, and controlling the temperature at-130 ℃ to obtain chromium powder;
s2 powder mixing: adding a deoxidizer into the chromium powder in the step S1, wherein the addition proportion is 0.7 wt%, and keeping the materials uniformly mixed to obtain mixed powder; wherein the deoxidizer is graphite powder;
s3 pressing: filling the mixed powder obtained in the step S2 into a mold, and pressing the mixed powder into a blank block by compression molding to obtain a chromium blank, wherein the pressure parameter is 15 MPa;
s4 sintering: putting the chromium blank obtained in the step S3 into a vacuum sintering furnace for sintering to obtain a sintered chromium blank, wherein the sintering temperature is controlled at 1350 ℃, the heat preservation time is 230 min, and the vacuum degree is 90 Pa; then closing the vacuum sintering furnace, and naturally cooling the chromium blank to room temperature in the furnace after sintering in the argon atmosphere;
s5 powder preparation: and (5) carrying out low-temperature grinding and crushing on the sintered chromium blank in the step (S4) to prepare powder, introducing liquid nitrogen as a protective medium, and controlling the temperature at-120 ℃ to obtain the low-hydrochloric-acid insoluble metal chromium powder.
Example 2
A preparation method of low-hydrochloric-acid-insoluble metal chromium powder comprises the following steps:
s1 preparation of chromium powder: grinding and crushing the chromium blocks at low temperature to prepare powder, introducing liquid nitrogen as a protective medium, and controlling the temperature at-130 ℃ to obtain chromium powder;
s2 powder mixing: adding a deoxidizer into the chromium powder in the step S1, wherein the addition proportion is 0.1 wt%, and keeping the materials uniformly mixed to obtain mixed powder; wherein the deoxidizer is graphite powder;
s3 pressing: filling the mixed powder obtained in the step S2 into a mold, and pressing the mixed powder into a blank block by compression molding to obtain a chromium blank, wherein the pressure parameter is 15 MPa;
s4 sintering: putting the chromium blank obtained in the step S3 into a vacuum sintering furnace for sintering to obtain a sintered chromium blank, wherein the sintering temperature is controlled at 1350 ℃, the heat preservation time is 230 min, and the vacuum degree is 95 Pa;
s5 powder preparation: and (5) carrying out low-temperature grinding and crushing on the sintered chromium blank in the step (S4) to prepare powder, introducing liquid nitrogen as a protective medium, and controlling the temperature at-120 ℃ to obtain the low-hydrochloric-acid insoluble metal chromium powder.
Example 3
A preparation method of low-hydrochloric-acid-insoluble metal chromium powder comprises the following steps:
s1 preparation of chromium powder: grinding and crushing the chromium blocks at low temperature to prepare powder, introducing liquid nitrogen as a protective medium, and controlling the temperature at-130 ℃ to obtain chromium powder;
s2 powder mixing: adding a deoxidizer into the chromium powder in the step S1, wherein the addition proportion is 1 wt%, and uniformly mixing the materials to obtain mixed powder; wherein the deoxidizer is graphite powder;
s3 pressing: filling the mixed powder obtained in the step S2 into a mold, and pressing the mixed powder into a blank block by compression molding to obtain a chromium blank, wherein the pressure parameter is 15 MPa;
s4 sintering: putting the chromium blank obtained in the step S3 into a vacuum sintering furnace for sintering to obtain a sintered chromium blank, wherein the sintering temperature is controlled at 1350 ℃, the heat preservation time is 230 min, and the vacuum degree is 80 Pa;
s5 powder preparation: and (5) carrying out low-temperature grinding and crushing on the sintered chromium blank in the step (S4) to prepare powder, introducing liquid nitrogen as a protective medium, and controlling the temperature at-120 ℃ to obtain the low-hydrochloric-acid insoluble metal chromium powder.
Example 4
This example is substantially the same as example 1, except that the sintering in step S4 is specifically as follows:
1) putting the chromium blank pressed in the step S3 into a vacuum sintering furnace with the vacuum degree of 85 Pa, heating to 480 ℃ at the speed of 5 ℃/min, and keeping the temperature for 25 min;
2) heating to 850 deg.C at a rate of 10 deg.C/min from 480 deg.C, maintaining for 20 min;
3) raising the temperature from 850 ℃ to 1350 ℃ at the speed of 5 ℃/min, and keeping the temperature for 230 min.
Example 5
This example is substantially the same as example 1, except that the mixed powder was packed into the mold in a layered packing manner before pressing in step S3,
the layered filling mode specifically comprises the following steps:
1) uniformly spraying the mixed powder obtained in the step S2 into a die through a powder sprayer, and continuously accumulating the thickness of the mixed powder to form a mixed powder layer, wherein the thickness of the mixed powder layer is 1.5 mm, and the uniformly spraying dosage on the mixed powder layer is 7 ml/cm2The deoxygenation liquid of (1);
2) subsequent pulse laser emissionA laser beam is emitted, the laser beam is focused into a laser band through a laser focusing system, the mixed powder layer is rapidly irradiated from left to right through the laser band to be slightly melted, and the surface density of the mixed powder layer is controlled to be 65%, wherein the laser energy density is 8 mJ/mm2The distance between the laser band and the surface of the mixed powder layer is 40 mm, and the sweeping speed of the laser band is 1.5 cm/s;
3) after laser beam scanning, the surface is quickly and uniformly sprayed with the spray dose of 7 ml/cm2Reducing the surface temperature of the deoxidizing liquid to 15 ℃;
4) repeating the steps 1) -3) for multiple times until the mixed powder is completely filled into a mold, and then performing compression molding to obtain a blank block to obtain a chromium blank;
wherein, the deoxygenation liquid in the step 1) and the step 3) consists of 13 parts of graphite powder, 3 parts of polyethylene glycol, 1 part of hydroxypropyl methyl cellulose and 27 parts of ethanol in parts by weight; wherein the particle size of the graphite powder is 0.02 mm;
the preparation method of the deoxygenation liquid comprises the following steps: adding graphite powder into water, continuously stirring, sequentially dropwise adding polyethylene glycol and hydroxypropyl methyl cellulose, and continuously stirring to obtain suspension, wherein the deoxygenation solution is required to be prepared and used as it is, and is required to be uniformly stirred before use.
Example 6
This example is substantially the same as example 5 except that the laser energy density in step 2) was 6 mJ/mm2The distance between the laser belt and the surface of the mixed powder layer is 35 mm, and the sweeping speed of the laser belt is 1 cm/s.
Example 7
This example is substantially the same as example 5 except that the laser energy density in step 2) was 9 mJ/mm2The distance between the laser band and the surface of the mixed powder layer is 45 mm, and the sweeping speed of the laser band is 2 cm/s.
Example 8
This example is substantially the same as example 1, except that sintering of S4: and (5) putting the chromium blank obtained in the step (S3) into a vacuum sintering furnace for sintering to obtain a sintered chromium blank, wherein the sintering temperature is controlled at 1000 ℃, the heat preservation time is 230 min, and the vacuum degree is 90 Pa.
Example 9
This example is substantially the same as example 1, except that sintering of S4: and (5) loading the chromium blank obtained in the step (S3) into a vacuum sintering furnace for sintering to obtain a sintered chromium blank, wherein the sintering temperature is controlled at 1500 ℃, the heat preservation time is 230 min, and the vacuum degree is 90 Pa.
Example 10
This example is substantially the same as example 1, except that sintering of S4: and (5) loading the chromium blank obtained in the step (S3) into a vacuum sintering furnace for sintering to obtain a sintered chromium blank, wherein the sintering temperature is controlled at 1350 ℃, the heat preservation time is 30 min, and the vacuum degree is 90 Pa.
Example 11
This example is substantially the same as example 1, except that sintering of S4: and (5) putting the chromium blank obtained in the step (S3) into a vacuum sintering furnace for sintering to obtain a sintered chromium blank, wherein the sintering temperature is controlled at 1350 ℃, the heat preservation time is 480 min, and the vacuum degree is 90 Pa.
Example 12
This example is substantially the same as example 1, except that the temperature of the low-temperature ground and pulverized powders in S1 and S5 was controlled at-150 ℃.
Example 13
This example is substantially the same as example 1 except that the temperature of the low-temperature ground and pulverized material in S1 and S5 was controlled to 0 ℃.
Determination test of insoluble hydrochloric acid in chromium powder
Firstly, test grouping: selecting untreated chromium powder as a control test, and recording as a control example; the chromium powder prepared by the preparation method of the above embodiment 1 to 7 is selected and recorded as experiment example 1, experiment example 2, experiment example 3, experiment example 4, experiment example 5, experiment example 6 and experiment example 7 in sequence;
the detection method comprises the following steps: the detection method refers to GB/T223.34-2000 'determination of insoluble hydrochloric acid in iron powder by chemical analysis method of steel and alloy';
the chromium powders prepared in the examples were measured in 3 groups according to the above groups and the detection method, and the average value of the measured values of the 3 groups was taken as the content of the insoluble hydrochloric acid in the chromium powder of the experimental example or the control example, and the measurement results are shown in the following table 1:
TABLE 1 table for determining content of insoluble hydrochloric acid in chromium powder of each group
| Examples of the experiments | Content of hydrochloric acid insoluble matter/%) |
| Experimental example 1 | 0.09 |
| Experimental example 2 | 0.11 |
| Experimental example 3 | 0.10 |
| Experimental example 4 | 0.08 |
| Experimental example 5 | 0.05 |
| Experimental example 6 | 0.06 |
| Experimental example 7 | 0.06 |
| Comparative example | 0.22 |
And (4) experimental conclusion:
1) in comparison with the comparative examples in experimental examples 1 to 7, the content of the insoluble hydrochloric acid in the chromium powder prepared in examples 1 to 7 was much lower than that in the untreated chromium powder in the comparative example, and it can be seen from the comparison of the data in table 1 that the content of the insoluble hydrochloric acid in the chromium powder can be effectively reduced by the preparation method of the present invention.
2) The comparison of experimental examples 1 to 3, and the difference between experimental examples 1, 2 and 3 lies in the difference of the content of graphite powder as deoxidizer, and it can be seen from the comparison of data in table 1 that the difference of the content of graphite powder as deoxidizer has a certain influence on the content of insoluble hydrochloric acid in the prepared chromium powder, wherein the content of insoluble hydrochloric acid in the chromium powder prepared by adding graphite powder as deoxidizer in the proportion of 0.7% of the total mass of chromium powder in example 1 is the lowest.
3) Compared with the experimental example 4, the experimental example 1 is different from the experimental example 4 in that the sintering method is different, the temperature of the experimental example 1 is directly increased to 1350 ℃, and the temperature of the experimental example 4 is increased to 1350 ℃ in a gradient manner, as can be seen from the comparison of the data in the table 1, the content of the hydrochloric acid insoluble substances of the chromium powder prepared in the experimental example 4 is lower than that of the chromium powder prepared in the experimental example 1, and therefore, the change of the sintering mode has certain influence on the content of the hydrochloric acid insoluble substances.
4) Compared with the experimental example 5, the experimental example 1 is different from the experimental example 5 in that the experimental example 1 adopts direct powder filling before pressing, and the experimental example 5 adopts layered powder filling for mixed powder filling, and as can be seen from comparison of data in table 1, the content of the insoluble hydrochloric acid in the chromium powder prepared in the experimental example 5 is lower than that of the chromium powder in the experimental example 1, and thus, the filling method in the experimental example 5 also has certain influence on the content of the insoluble hydrochloric acid.
5) Experimental examples 5 to 7, and experimental examples 5, 6 and 7 were different in the difference of the laser slightly melting treatment parameters in step 2), and it can be seen from the comparison of the data in table 1 that the difference of the laser slightly melting parameters has a certain influence on the content of the insoluble hydrochloric acid in the prepared chromium powder, wherein the content of the insoluble hydrochloric acid in the chromium powder prepared under the laser slightly melting parameters in example 5 is the lowest.
Second, the sintering temperature and time were investigated by selecting the above examples 1 and 8 to 11, and the examples are described as experiment 1 and 8 to 11, and the details are as follows:
the chromium powders prepared in examples 8 to 11 were each subjected to the content of insoluble matter in hydrochloric acid by the above-mentioned method, and the results were as follows:
TABLE 2 table for measuring content of insoluble hydrochloric acid in chromium powder of Experimental examples 1 and 8-11
| Examples of the experiments | Content of hydrochloric acid insoluble matter/%) |
| Experimental example 1 | 0.090 |
| Experimental example 8 | 0.097 |
| Experimental example 9 | 0.094 |
| Experimental example 10 | 0.093 |
| Experimental example 11 | 0.091 |
And (4) conclusion: in comparison with the above example 1, the sintering temperatures of the above examples 8-9 and 1 are different, and it can be seen from the above table 2 that the sintering temperature has a certain effect but is not large on the content of hydrochloric acid insoluble matter, wherein the content of hydrochloric acid insoluble matter in chromium powder prepared at the sintering temperature of the above example 1 is the lowest; compared with the experimental example 1, the heat preservation time of the sintering of the experimental examples 10-11 is different from that of the experimental example 1, and the heat preservation time of the sintering has lower influence on the content of the hydrochloric acid insoluble substances as can be seen from the table 2, wherein the content of the chromium powder hydrochloric acid insoluble substances prepared under the heat preservation time of the sintering in the experimental example 1 is the lowest;
thirdly, the low-temperature grinding and crushing pulverization temperatures are researched by selecting the experimental example 1 and the experimental examples 12-13, which are recorded as the experimental example 1 and the experimental examples 12-13, and the concrete steps are as follows:
TABLE 3 table for measuring content of insoluble hydrochloric acid in chromium powder of Experimental examples 1 and 12-13
| Examples of the experiments | Content of hydrochloric acid insoluble matter/%) |
| Experimental example 1 | 0.090 |
| Experimental example 12 | 0.090 |
| Experimental example 13 | 0.091 |
And (4) conclusion: in comparison with experiment 1, experiment 12-13 has different temperature for milling by low temperature grinding and crushing, and table 3 shows that the temperature for milling by low temperature grinding and crushing has almost no influence, wherein the chromium powder prepared by experiment 1 and experiment 12 has the lowest content of hydrochloric acid insoluble matter, and the data of experiment 1 is selected as the parameters for milling by low temperature grinding and crushing in consideration of the problems of detection precision, low temperature control cost, and the like.
Claims (5)
1. A preparation method of low-hydrochloric-acid-insoluble metal chromium powder is characterized by comprising the following steps:
s1 preparation of chromium powder: grinding and crushing the chromium blocks at low temperature to prepare powder, and controlling the temperature to be-150-0 ℃ to obtain chromium powder;
s2 powder mixing: adding a deoxidizer into the chromium powder in the step S1, wherein the addition proportion accounts for 0.1-5 wt% of the total amount of the chromium powder, and keeping the materials uniformly mixed to obtain mixed powder;
s3 pressing: filling the mixed powder obtained in the step S2 into a mould in a layered manner, and specifically comprising the following steps:
1) uniformly spraying the mixed powder obtained in the step S2 into a die through a powder sprayer, and continuously accumulating the thickness of the mixed powder to form a mixed powder layer, wherein the thickness of the mixed powder layer is 1-2 mm, and the uniformly spraying dosage on the mixed powder layer is 5-10 ml/cm2The deoxygenation liquid of (1);
2) then, a pulse laser emits a laser beam, the laser beam is focused into a laser line or a laser band through a laser focusing system, the mixed powder layer is rapidly irradiated from left to right through scanning of the laser line or the laser band to be slightly melted, and the surface density of the mixed powder layer is controlled to be 50-70%, wherein the laser energy density is 6-9 mJ/mm2The distance between the laser line or the laser band and the surface of the mixed powder layer is 35-45 mm, and the sweeping speed of the laser line or the laser band is 1-2 cm/s;
3) after laser beam scanning, the surface is quickly and uniformly sprayed with 5-10 ml/cm of spray dosage2Reducing the surface temperature of the deoxidizing liquid to 10-15 ℃;
4) repeating the steps 1) -3) for multiple times until the mixed powder is completely filled into a mold, and then performing compression molding to form a blank block to obtain a chromium blank, wherein the pressure parameter is 5-20 MPa;
s4 sintering: putting the chromium blank obtained in the step S3 into a vacuum sintering furnace for sintering to obtain a sintered chromium blank;
s5 powder preparation: carrying out low-temperature grinding and crushing on the sintered chromium blank in the step S4 to prepare powder, and controlling the temperature to be-150-0 ℃ to obtain low-hydrochloric-acid-insoluble metal chromium powder;
the deoxidizer is graphite powder;
the deoxygenation liquid in the step 1) and the step 3) comprises, by weight, 10-15 parts of graphite powder, 2-3 parts of polyethylene glycol, 1-2 parts of hydroxypropyl methyl cellulose and 20-30 parts of ethanol; wherein the particle size of the graphite powder is 0.02-0.05 mm.
2. The method for preparing low-hydrochloric-acid-insoluble metallic chromium powder according to claim 1, wherein the sintering temperature in the sintering in step S4 is controlled to be 1000-1500 ℃, the heat preservation time is 30-480 min, and the vacuum degree is less than 100 Pa.
3. The method for preparing low hydrochloric acid insoluble metal chromium powder according to claim 1, wherein the sintering in step S4 is specifically as follows:
1) putting the chromium blank obtained in the step S3 into a vacuum sintering furnace with the vacuum degree less than 100 Pa, heating to 450-550 ℃ at the speed of 5 ℃/min, and keeping the temperature for 10-30 min;
2) heating to 800-900 ℃ from 450-550 ℃ at a speed of 10 ℃/min, and keeping the temperature for 10-30 min;
3) raising the temperature from 800-900 ℃ at a speed of 5 ℃/min to 1000-1500 ℃, and keeping the temperature for 30-480 min.
4. The method for preparing low hydrochloric acid insoluble metallic chromium powder as claimed in claim 1, wherein the low temperature grinding and crushing powder in steps S1 and S5 both use liquid nitrogen as protective medium.
5. The method for preparing low hydrochloric acid insoluble metal chromium powder according to claim 1, wherein the cooling treatment after sintering in step S4 is specifically: and closing the vacuum sintering furnace, and naturally cooling the sintered chromium blank in the furnace to room temperature in an argon atmosphere.
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